CN211050938U - Continuous refined apparatus for producing of dimethyl phosphite - Google Patents
Continuous refined apparatus for producing of dimethyl phosphite Download PDFInfo
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- CN211050938U CN211050938U CN201921835148.1U CN201921835148U CN211050938U CN 211050938 U CN211050938 U CN 211050938U CN 201921835148 U CN201921835148 U CN 201921835148U CN 211050938 U CN211050938 U CN 211050938U
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Abstract
The utility model provides a dimethyl phosphite continuous refining production device, wherein the top of a low-boiling removal tower is connected with a feeding preheater, the feeding preheater is connected with a low-boiling removal tower condenser, the low-boiling removal tower condenser is connected with a low-boiling removal tower buffer tank, and the low-boiling removal tower buffer tank is connected with the low-boiling removal tower through a low-boiling removal tower reflux pump; the low-boiling removal tower is connected with a high-boiling removal tower through a low-boiling removal tower discharge pump, and a condenser at the top of the high-boiling removal tower is connected; the first-stage condenser of the high-boiling removal tower and the second-stage condenser of the high-boiling removal tower are respectively connected with a buffer tank of the high-boiling removal tower. The device utilizes the existing dimethyl phosphite crude ester rectification production technology, solves the uncontrollable links in many aspects in the dimethyl phosphite batch rectification production process, improves the utilization rate of the crude ester by 2 percent, reduces the content of dimethyl phosphite in the still residual liquid by within 5 percent, increases the dimethyl phosphite by 3250 tons/year, saves the steam unit consumption by 1.5 tons/ton, and has obvious economic benefit.
Description
Technical Field
The utility model relates to a dimethyl phosphite apparatus for producing, concretely relates to dimethyl phosphite serialization rectification production technology, through two rectifying column series connected modes respectively the desorption low boiling thing (methyl alcohol and chloromethane) and high boiling thing (methyl phosphite, dimethyl phosphite, phosphorous acid, all the other are some high boiling thing that contain P-O-P bond) to realize that dimethyl phosphite's serialization is refined.
Background
Dimethyl phosphite is an important chemical raw material and intermediate, is widely applied to the preparation industries of organic phosphonic acid type corrosion inhibitors, synthetic plastic additives, dye additives, combustion improvers and pesticides, and is an important intermediate for preparing organic phosphorus pesticides such as trichlorphon, dichlorvos, fenoxanil, omethoate, glyphosate and the like.
In 2016, the yield of glyphosate in China is about 48 ten thousand tons, which accounts for more than 50% of the global yield of glyphosate and jumps the first world. With the increasingly fierce competition of the glyphosate industry, the glyphosate is industrially continuously synthesized by adopting a spraying and hedging reaction mode, phosphorus trichloride and methanol are mixed in a hedging pipe according to a certain proportion to rapidly react to produce dimethyl phosphite, a large amount of heat is released, by-product hydrogen chloride and methyl chloride gas in the reaction process are rapidly pumped away through vacuum, further side reaction between the hydrogen chloride and the dimethyl phosphite is avoided, in order to reduce the generation of the side reaction, the material after the esterification reaction is further heated for deacidification, cooling water is filled in a jacket of an esterification kettle to remove the reaction heat, and the reaction is kept to be carried out stably. The demand of dimethyl phosphite as an important intermediate for producing glyphosate is also increased sharply, the traditional batch rectification process faces a serious challenge and cannot meet the existing production demand, and the crude ester (the content can reach 82%) obtained after continuous deacidification after esterification contains low-boiling-point substances of methanol and high-boiling-point substances such as byproduct monomethyl phosphite, phosphorous acid and the like, but because the reaction product composition is complex, the mixture has high boiling point, strong corrosivity and great separation difficulty, the product refining (the content is larger than or equal to 96.5 percent and the acidity is smaller than or equal to 0.15 percent) is still continuously carried out by batch reduced pressure rectification. The rectification method has high energy consumption, low processing capacity and numerous and complicated equipment, and is difficult to adapt to large-scale industrial production.
In the esterification reaction of dimethyl phosphite, byproducts such as methyl chloride, phosphorous acid and the like are generated, so that a crude product to be separated contains various components such as raw materials of methyl alcohol, methyl chloride, phosphorous acid, hydrochloric acid and the like, and the acid value of dimethyl phosphite is reduced. Wherein the boiling point of methyl chloride is-23.73 ℃, the boiling point of methanol is 64.7 ℃, the boiling point of dimethyl phosphite is 171 ℃, and the boiling point of phosphorous acid is 200 ℃.
At present, a batch method rectification technology is adopted for rectifying the dimethyl phosphite crude ester of the company, light components such as dimethyl phosphite, methanol and the like are extracted from the top of a tower in a single-tower rectification mode, and products are collected by the light components in circulating water condensation and frozen brine condensation modes.
But the single-tower rectification time is long, the labor intensity of workers is high, the product quality is unstable, the product yield is low, the energy consumption for separation is high and the like, the production capacity of the device is limited to a certain extent, and the increasing requirements of the current market and companies are difficult to meet.
Disclosure of Invention
Problems with batch rectification: 1. the intermittent rectification increases the azeotropic temperature along with the increase of the concentration of the residue in the kettle, and the evaporation area is not correspondingly increased, so the temperature of the kettle of the tower needs to be continuously increased to ensure the evaporation capacity of the product and the top discharge of the main fraction, and the long-time high-temperature boiling process can cause side reaction (the decomposition of dimethyl phosphite), thereby causing the instability of yield and quality; 2. the operation condition fluctuates, along with the continuous operation of the batch type rectification, heavy components in the tower kettle are gradually accumulated, the kettle temperature and the top temperature are firstly low and then high, and certain influence is brought to the stability of the product quality; 3. the method has the defects of easy corrosion of equipment and large equipment maintenance and replacement amount, and the main reason is that the crude product liquid contains phosphorous acid, and the higher the temperature is, the higher the corrosivity of the equipment is; 4. the automation control is low, the productivity efficiency of the equipment is not high, and the energy consumption is large.
The utility model discloses the device is promptly for utilizing current dimethyl phosphite crude ester rectification production technology, bold innovation in the aspect of crude ester rectification process equipment, investigation and demonstration repeatedly, many-sided uncontrollable link in the solution dimethyl phosphite batch type rectification production process, the energy consumption is high, product acid value is high, cauldron raffinate dimethyl phosphite content high grade and so on technological problem, the security of production technology and system has been guaranteed, the utilization ratio 2% of crude ester has been improved, product quality is improved, it reaches within 5% to reduce dimethyl phosphite content in the cauldron raffinate, increase dimethyl phosphite 3250 ton/year, practice thrift steam unit consumption 1.5 ton/ton, economic benefits is showing, the continuous refining technology of while adoption has improved workman's operational environment greatly, the intensity of labour has been alleviateed, and the labor efficiency is improved. The continuous rectification adopts vacuum operation, the device has no leakage, zero emission, environmental protection and accordance with the requirement of green development.
Aiming at the problems existing in the prior batch type rectification technology, the utility model provides a dimethyl phosphite continuous rectification device. The continuous rectification of dimethyl phosphite is realized by using a continuous rectification mode under reduced pressure and respectively removing low-boiling-point substances (methanol and methyl chloride) and high-boiling-point substances (monomethyl phosphite, dimethyl phosphite and phosphorous acid, and the rest are high-boiling-point substances containing P-O-P bonds) in a serial mode of two rectification towers. Distilling low-boiling-point substances from the top of the first tower, further separating the discharged liquid from the bottom of the tower in a second tower, distilling high-purity dimethyl phosphite from the top of the tower, and taking the residual liquid in the bottom of the tower as high-boiling-point substances. In order to realize the purpose of the utility model, the utility model adopts the following technical scheme:
a dimethyl phosphite continuous refining production device is characterized in that a dimethyl phosphite pipeline is connected with a feeding preheater through a crude ester feeding pump, the feeding preheater is connected with a low-boiling-point removal tower, the top of the low-boiling-point removal tower is connected with the feeding preheater, the feeding preheater is connected with a low-boiling-point removal tower condenser, the low-boiling-point removal tower condenser is connected with a low-boiling-point removal tower buffer tank, and the low-boiling-point removal tower buffer tank is connected with the low-boiling-point removal tower through a low-boiling-point removal tower reflux pump;
the low-boiling removal tower is connected with a high-boiling removal tower through a low-boiling removal tower discharge pump, the top of the high-boiling removal tower is connected with a first-stage condenser of the high-boiling removal tower, and the top of the first-stage condenser of the high-boiling removal tower is connected with the bottom of a second-stage condenser of the high-boiling removal tower;
the high-boiling-point-removing tower primary condenser and the high-boiling-point-removing tower secondary condenser are respectively connected with a high-boiling-point-removing tower buffer tank, and the high-boiling-point-removing tower buffer tank is connected to a dimethyl phosphate discharging area through a high-boiling-point-removing tower reflux pump.
The bottom of the low-boiling tower is connected with a reboiler of the low-boiling tower through a forced circulation pump of the low-boiling tower, and the reboiler of the low-boiling tower is connected with the low-boiling tower to form a circulation loop.
The low-boiling-point removal tower buffer tank is also connected to a methanol storage tank through a low-boiling-point removal tower reflux pump.
The bottom of the high-boiling-point removal tower is connected with a reboiler of the high-boiling-point removal tower through a forced circulation pump of the high-boiling-point removal tower, and the reboiler of the high-boiling-point removal tower is connected with the high-boiling-point removal tower to form a circulation loop.
The high-boiling-point removal tower buffer tank is also connected with the high-boiling-point removal tower through a high-boiling-point removal tower reflux pump.
And (3) carrying out mass transfer heat exchange on the methanol and the chloromethane light components extracted from the top of the low-boiling removal tower and the crude ester fed by a crude ester feeding pump through a feeding preheater, and preliminarily condensing the methanol and the chloromethane light components.
The low-boiling-point removal tower condenser is connected with a low-boiling-point removal tower buffer tank and a low-boiling-point removal tower vacuum pump, light component liquid obtained by continuously condensing light components of methanol and chloromethane through frozen brine in a secondary mode enters the low-boiling-point removal tower buffer tank, and the low-boiling-point removal tower buffer tank is connected with a low-boiling-point removal tower reflux pump to form light component reflux and extraction. The vacuum pump of the low-boiling removal tower provides negative pressure conditions for the low-boiling removal tower system, the temperature of the tower kettle system is reduced, methanol and methyl chloride light components are subjected to secondary condensation of frozen brine to obtain methanol, non-condensable gas methyl chloride is collected and then enters a tail gas treatment system of a crude ester production system, and the collected non-condensable gas methyl chloride enters a power system and a methyl chloride recovery system to recover methyl chloride after being absorbed by a concentrated acid tower, absorbed by a dilute acid tower and washed by a washing tower.
The forced circulation pump of the high-boiling tower is connected with a reboiler of the high-boiling tower, the reboiler of the high-boiling tower provides heat for the mixed solution of dimethyl phosphite and phosphorous acid, the mixed solution of dimethyl phosphite and phosphorous acid extracted from the bottom of the low-boiling tower is heated to be partially vaporized through the reboiler of the high-boiling tower, and the mixed solution enters a high-boiling rectifying tower in a vapor-liquid mixture state for further rectification.
The high-purity dimethyl phosphite vapor distilled from the tower top is secondarily condensed into liquid through circulating water and frozen brine, one part of the liquid is returned to the high-boiling tower as reflux, and the other part of the liquid is used as a product and is fed into a dimethyl phosphite finished product tank. The vacuum pump of the high-boiling removal tower provides negative pressure conditions for the high-boiling removal tower system, and reduces the temperature of the tower kettle system. The tower kettles of the two rectifying towers adopt common medium-pressure steam as a heating agent.
And discharging the high-boiling residues discharged from the bottom of the high-boiling rectification tower to a high-boiling residue storage tank through a high-boiling residue discharging pump.
Advantageous effects
The technical scheme ensures the safety of a production process and a production system, improves the utilization rate of active ingredients of the crude ester, improves the quality and stability of the product of the crude ester by using a control method of maintaining constant reflux quantity at the top of the tower through fixed value control of a regulating valve, reduces the content of dimethyl phosphite in the residual liquid in the kettle, can save 1.5 tons/ton of steam consumption by carrying out mass transfer and heat exchange on a gas-phase light component extracted from the top of the low-boiling tower and a crude ester feeding liquid-phase component, and has remarkable economic benefit.
Drawings
FIG. 1 is a schematic structural diagram of a continuous refining production apparatus for dimethyl phosphite, wherein 1, a reboiler of a low-boiling removal tower, 2, a feed preheater, 3, a low-boiling removal tower, 4, a buffer tank of the low-boiling removal tower, 5, a condenser of the low-boiling removal tower, 6, a high-boiling removal tower, 7, a reboiler of the high-boiling removal tower, 8, a buffer tank of the high-boiling removal tower, 9, a first-stage condenser of the high-boiling removal tower, 10, a second-stage condenser of the high-boiling removal tower, 11, a forced circulation pump of the low-boiling removal tower, 12, a discharge pump of the low-boiling removal tower, 13, a crude ester feed pump, 14, a reflux pump of the low-boiling removal tower, 15, a vacuum pump of the low-boiling removal tower, 16, a forced circulation pump of the high-boiling removal tower, 17, a.
Detailed Description
Example 1
A dimethyl phosphite continuous refining production device is characterized in that a dimethyl phosphite pipeline is connected with a feeding preheater 2 through a crude ester feeding pump 13, the feeding preheater 2 is connected with a low-boiling-point removal tower 3, the top of the low-boiling-point removal tower 3 is connected with the feeding preheater 2, the feeding preheater 2 is connected with a low-boiling-point removal tower condenser 5, the low-boiling-point removal tower condenser 5 is connected with a low-boiling-point removal tower buffer tank 4, and the low-boiling-point removal tower buffer tank 4 is connected with the low-boiling-point removal tower 3 through a low-boiling-point removal tower reflux pump 14;
the low-boiling removal tower 3 is connected with a high-boiling removal tower 6 through a low-boiling removal tower discharge pump 12, the top of the high-boiling removal tower 6 is connected with a first-stage condenser 9 of the high-boiling removal tower, and the top of the first-stage condenser 9 of the high-boiling removal tower is connected with the bottom of a second-stage condenser 10 of the high-boiling removal tower;
the high-boiling-point-removing tower primary condenser 9 and the high-boiling-point-removing tower secondary condenser 10 are respectively connected with a high-boiling-point-removing tower buffer tank 8, and the high-boiling-point-removing tower buffer tank 8 is connected to a dimethyl phosphate discharging area through a high-boiling-point-removing tower reflux pump 18.
The bottom of the low-boiling-point removal tower 3 is connected with a low-boiling-point removal tower reboiler 1 through a low-boiling-point removal tower forced circulation 11, and the low-boiling-point removal tower reboiler 1 is connected with the low-boiling-point removal tower 3 to form a circulation loop.
The low-boiling-point removal tower buffer tank 4 is also connected to a methanol storage tank through a low-boiling-point removal tower reflux pump 14.
The bottom of the high-boiling-point removal tower 6 is connected with a high-boiling-point removal tower reboiler 7 through a high-boiling-point removal tower forced circulation pump 16, and the high-boiling-point removal tower reboiler 7 is connected with the high-boiling-point removal tower 6 to form a circulation loop.
The high-boiling-point removal tower buffer tank 8 is also connected with the high-boiling-point removal tower 6 through a high-boiling-point removal tower reflux pump 18.
And the low-boiling-point-removing tower reboiler 1 and the high-boiling-point-removing tower reboiler 7 are respectively provided with a steam inlet and outlet pipeline.
And condensed brine inlet and outlet pipelines are arranged on the low-boiling-point-removing tower condenser 5, the high-boiling-point-removing tower first-stage condenser 9 and the high-boiling-point-removing tower second-stage condenser 10.
Description of the drawings: the crude ester sent from the esterification deacidification procedure firstly enters a low-boiling-point-removing rectifying tower for rectification. The low-boiling-point substance steam pre-distilled in the tower is condensed into liquid (methanol) and non-condensable gas (chloromethane) by a condensing cooler, one part of the low-boiling-point substance steam is returned to the low-boiling-point removal tower as reflux, and the other part of the low-boiling-point substance steam is taken as a distilled product and enters a low-boiling-point substance storage tank. The liquid discharged from the bottom of the low-boiling tower enters an intermediate tank, is heated by a preheater until being partially vaporized, and enters a high-boiling rectification tower in a vapor-liquid mixture state for further rectification. High-purity dimethyl phosphite vapor distilled from the tower top is condensed into liquid by a condensing cooler, one part of the liquid is returned to the high-boiling tower as reflux, and the other part of the liquid is taken as a product and is put into a dimethyl phosphite finished product tank. The liquid discharged from the bottom of the high-boiling tower enters a high-boiling substance storage tank and can be further processed to produce phosphorous acid.
Example 2
The control method of the dimethyl phosphite continuous rectification system comprises a low-boiling-point substance removal process and a refining process, and the continuous refining processing capacity is 4 tons/hour in the embodiment.
The low-boiling-point substance removing process comprises the following steps: putting the dimethyl phosphite crude product into a crude product storage tank, feeding from the middle part of a low-boiling substance removal tower, starting a crude ester feeding pump 13, feeding into a low-boiling substance removal tower 3, slowly opening a feeding flowmeter automatic valve, adjusting the flow (the feeding flow is 0.5-4 tons/hour in normal operation), closely paying attention to the liquid level in the low-boiling substance removal tower kettle, and gradually reducing the feeding amount when the liquid level of the low-boiling substance removal tower reaches 60%. Carrying out vacuum and temperature rise, starting a vacuum pump 15 of the light component removal tower, carrying the vacuum of the light component removal tower 3 to more than-95 kPa, opening a hydrophobic bypass valve of the light component removal tower, completely discharging condensed water in a coil, opening front and rear valves of a steam regulating valve of a reboiler 1 of the light component removal tower, manually setting the steam regulating valve, regulating the opening degree of a steam flow regulating valve by taking steam pressure and material temperature in the light component removal tower kettle as reference indexes, closing the hydrophobic bypass valve after the condensed water is completely discharged, paying attention to the liquid level of the tower kettle 3 of the light component removal tower, and replenishing raw materials according to the liquid level condition. And (4) performing total reflux at the initial stage of low boiling removal, closing a material ejection valve of the light component removal tower, fully opening a reflux valve, and keeping the total reflux state for more than 30 minutes. The steam flow and the temperature at the top of the tower are controlled in a linkage way, the steam flow is adjusted according to the pressure difference between the top of the tower and the bottom of the tower, the steam pressure and the temperature in the kettle, the steam pressure is controlled to be 0-0.6MPa, the temperature of the kettle of the light component removal tower is 80 ℃, the temperature of the top of the tower is 50 ℃, and the pressure difference between the top of the tower and the kettle of the tower is more. After continuous reflux is stabilized for half an hour, liquid level and temperature in a light component removal tower kettle 3 are taken as references, a small amount of dimethyl phosphite crude raw material is continuously fed into a low boiling tower, the temperature of the kettle in the kettle reaches more than 80 ℃ and the kettle bottom sampling is qualified, a kettle bottom discharge valve is opened, a discharge pump 12 is started to convey the material to a high boiling tower 6, the liquid level of a buffer tank 4 of the low boiling tower is subjected to linkage control with a discharge regulating valve, a tower top discharge valve is opened, the discharge amount is controlled according to the tower top sampling and the tower kettle sampling, the tower top discharge is controlled at 3 tons/hour, the feeding amount is gradually increased, after the parameters of the whole tower are stabilized, a raw material feeding flow control valve, a reflux control valve, a reboiler temperature control valve of the low boiling tower is automatically controlled, and the.
The refining process comprises the following steps: starting a discharging pump 12 of the low-boiling removal tower, feeding into the high-boiling removal tower 6, slowly opening an automatic valve of a feed flow meter, adjusting the flow (controlling the flow at 3 tons/hour during normal operation), controlling the liquid level in the high-boiling removal tower 12, and reducing the feed flow when the liquid level reaches 60%. The method comprises the steps of vacuumizing and heating, starting a rectification vacuum pump 19, controlling the vacuum of a high-boiling tower to be more than-95 kPa, opening a drain bypass valve of a finished product tower, draining condensed water in a coil pipe, opening front and rear valves of a steam regulating valve of a reboiler of the high-boiling tower, manually setting the steam regulating valve, regulating the opening degree of a steam flow regulating valve according to steam pressure and material temperature in a kettle, closing the drain bypass valve after the condensed water is drained, paying attention to the liquid level of the high-boiling tower 12, and regulating the feeding flow according to the liquid level. And (3) performing total reflux, closing a discharge valve at the top of the tower, closing a discharge valve of a finished product, starting a reflux pump 18 of the high-boiling-point removal tower, opening a reflux valve, adjusting reflux flow, keeping the total reflux state for more than 30 minutes, adjusting the steam quantity according to the pressure difference between the top of the tower and the bottom of the tower, the steam pressure and the temperature in the kettle, controlling the temperature of the kettle of the tower to be 140 ℃, the temperature of the top of the tower to be 120 ℃, the pressure difference between the top of the tower and the kettle of the. Discharging, after the reflux is stable for half an hour, continuously feeding a small amount of raw materials into the high-boiling-point removal tower by taking the liquid level and the temperature in the tower kettle as the basis, controlling the reflux amount according to the instant sample of a finished product, setting the discharge control as automatic control (control of a regulating valve), gradually increasing the feeding amount, after the parameters of the whole tower are stable, automatically controlling a crude product feeding flow control valve, a reflux amount control valve and a reboiler temperature control valve, entering the normal operation process, paying attention to the temperature change of the tower kettle, keeping the temperature over 150 ℃, starting a high-boiling-point removal discharge pump 17, transferring tower kettle materials into a high-boiling-point storage tank, and sampling from the high-boiling-point pump at intervals after the discharge of the high-boiling-.
Claims (5)
1. A continuous refining production device of dimethyl phosphite is characterized in that a dimethyl phosphite pipeline is connected with a feeding preheater (2) through a crude ester feeding pump (13), the feeding preheater (2) is connected with a low-boiling-point removal tower (3), the top of the low-boiling-point removal tower (3) is connected with the feeding preheater (2), the feeding preheater (2) is connected with a low-boiling-point removal tower condenser (5), the low-boiling-point removal tower condenser (5) is connected with a low-boiling-point removal tower buffer tank (4), and the low-boiling-point removal tower buffer tank (4) is connected with the low-boiling-point removal tower (3) through a low-boiling-point removal tower reflux pump (14);
the low-boiling removal tower (3) is connected with a high-boiling removal tower (6) through a low-boiling removal tower discharge pump (12), the top of the high-boiling removal tower (6) is connected with a first-stage condenser (9) of the high-boiling removal tower, and the top of the first-stage condenser (9) of the high-boiling removal tower is connected with the bottom of a second-stage condenser (10) of the high-boiling removal tower;
the high-boiling-point-removing tower primary condenser (9) and the high-boiling-point-removing tower secondary condenser (10) are respectively connected with a high-boiling-point-removing tower buffer tank (8), and the high-boiling-point-removing tower buffer tank (8) is connected to a dimethyl phosphate discharging area through a high-boiling-point-removing tower reflux pump (18).
2. The continuous refining production device of dimethyl phosphite according to claim 1, wherein the bottom of the low-boiling tower (3) is connected with the reboiler (1) of the low-boiling tower through the forced circulation pump (11) of the low-boiling tower, and the reboiler (1) of the low-boiling tower is connected with the low-boiling tower (3) to form a circulation loop.
3. The continuous refining production device of dimethyl phosphite according to claim 1, wherein the buffer tank (4) of the low-boiling tower is further connected to a methanol storage tank through a reflux pump (14) of the low-boiling tower.
4. The continuous refining production device of dimethyl phosphite according to claim 1, wherein the bottom of the high boiling removal column (6) is connected with the reboiler (7) of the high boiling removal column through the forced circulation pump (16) of the high boiling removal column, and the reboiler (7) of the high boiling removal column is connected with the high boiling removal column (6) to form a circulation loop.
5. The continuous refining production apparatus of dimethyl phosphite according to claim 1, wherein the buffer tank (8) of the high-boiling removal tower is further connected with the high-boiling removal tower (6) through a reflux pump (18) of the high-boiling removal tower.
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