CN113617050A - Energy-saving BDO (BDO) rectifying device and method - Google Patents

Energy-saving BDO (BDO) rectifying device and method Download PDF

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Publication number
CN113617050A
CN113617050A CN202111184505.4A CN202111184505A CN113617050A CN 113617050 A CN113617050 A CN 113617050A CN 202111184505 A CN202111184505 A CN 202111184505A CN 113617050 A CN113617050 A CN 113617050A
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tower
boiling
condenser
circulating
salt
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夏君君
彭涛
全晓宇
尹海蛟
于会满
唐昊
刘莉
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Jiangsu Leke Energy Saving Technology Co ltd
Tianjin Leke Energy Saving Technology Co ltd
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Jiangsu Leke Energy Saving Technology Co ltd
Tianjin Leke Energy Saving Technology Co ltd
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Priority to CN202111184505.4A priority Critical patent/CN113617050A/en
Publication of CN113617050A publication Critical patent/CN113617050A/en
Priority to CN202220713998.XU priority patent/CN217367194U/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/06Flash distillation
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/80Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C31/00Saturated compounds having hydroxy or O-metal groups bound to acyclic carbon atoms
    • C07C31/18Polyhydroxylic acyclic alcohols
    • C07C31/20Dihydroxylic alcohols
    • C07C31/2071,4-Butanediol; 1,3-Butanediol; 1,2-Butanediol; 2,3-Butanediol
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals

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  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

The invention discloses an energy-saving BDO rectification device and a method, wherein cold material flow outlets of tower top condensers of a circulating tower and a concentrating tower are connected with an inlet of a compressor A, an outlet of the compressor A is respectively connected with heat source inlets of tower kettle reboilers of the circulating tower and the concentrating tower, a heat source outlet of the tower kettle reboiler of the circulating tower and a heat source outlet of the tower kettle reboiler of the concentrating tower are respectively connected with inlets of respective tower top condensers; the cold material flow outlets of the tower top condensers of the salt tower, the low-boiling tower and the high-boiling tower are connected with the inlet of a compressor B, the outlet of the compressor B is respectively connected with the heat source inlets of the tower kettle reboilers of the salt tower, the low-boiling tower and the high-boiling tower, the heat source outlet of the tower kettle reboilers of the salt tower, the heat source outlet of the tower kettle reboilers of the low-boiling tower and the heat source outlet of the tower kettle reboilers of the high-boiling tower are respectively connected with the inlets of the tower top condensers of the high-boiling tower. Compared with the prior art, the method saves a large amount of steam and circulating water, and can save about 68.7 percent of operation cost each year.

Description

Energy-saving BDO (BDO) rectifying device and method
Technical Field
The invention belongs to the technical field of energy conservation of rectification, and particularly relates to an energy-saving BDO rectification device and method.
Background
BDO (1, 4-butanediol) is an important organic chemical and fine chemical raw material, and can generate various derivatives such as THF, PTMEG, GBL and the like. BDO and the derivatives thereof can be widely applied to the fields of PBT plastics, spandex, polyurethane, pharmacy, cosmetics and the like. At present, the mainstream production technology is an aldyne method, namely acetylene and formaldehyde are used as raw materials, the raw materials react under the action of a catalyst in a reactor to generate 1, 4-Butynediol (BYD), meanwhile, byproducts such as water, methanol and the like are generated, the mixture is sent into a formaldehyde circulating tower, formaldehyde is recycled to a previous reaction section, and the mixture of the BYD and the water in a tower kettle enters a fine filtration system; after removing a catalyst by fine filtration, a mixture of BYD and water enters a hydrogenation reactor, BYD reacts to generate BDO, a hydrogenation product enters a concentration tower to remove moisture, and the BDO concentration is increased; high-concentration BDO enters a salt tower to remove salt, a mixture of BDO extracted from the tower top and water enters a low-boiling tower, low-boiling substances such as water and the like are removed from the tower top of the low-boiling tower, and tower kettle materials enter a high-boiling tower; a small amount of heavy components are extracted from the tower kettle of the high-boiling tower, a small amount of light components are extracted from the tower top, and a product BDO is extracted from the side line.
BDO is reported to be one of raw materials of degradable plastics, and the demand of BDO is rapidly increased along with the implementation of national plastic constraints. However, the energy consumption of BDO in the rectification production process is large, taking a BDO device of a certain chemical plant of 10 ten thousand tons/year as an example, the amount of steam consumed each year is about 77 ten thousand tons, and the single steam item consumed by the public engineering cost reaches 1.2 million yuan. Nowadays, the technology for producing BDO by an aldyne method in China is mature, and if the competitiveness of a product is further improved, the energy consumption cost of the product must be reduced.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide an energy-saving BDO rectifying device and method.
The invention is realized by the following technical scheme:
an energy-saving BDO rectifying device is characterized by comprising a catalytic reactor, a circulating tower, a hydrogenation reactor, a concentration tower, a salt tower, a low-boiling tower and a high-boiling tower, wherein an outlet of the catalytic reactor is connected with an inlet of the circulating tower, a tower bottom liquid outlet of the circulating tower is connected with an inlet of the hydrogenation reactor, an outlet of the hydrogenation reactor is connected with an inlet of the concentration tower, a tower bottom liquid outlet of the concentration tower is connected with an inlet of the salt tower, a material outlet of a tower top condenser of the salt tower is connected with a feed inlet of the low-boiling tower, a tower bottom liquid outlet of the low-boiling tower is connected with a feed inlet of the high-boiling tower, and a side draw outlet of the high-boiling tower is a product outlet of BDO;
the circulating tower, the concentration tower, the salt tower, the low-boiling tower and the high-boiling tower are all provided with a tower top condenser and a tower kettle reboiler,
cold material flow outlets of the condenser at the top of the circulating tower and the condenser at the top of the concentrating tower are both connected with an inlet of a compressor A, outlets of the compressor A are respectively connected with a tower kettle reboiler of the circulating tower and a heat source inlet of a tower kettle reboiler of the concentrating tower, a heat source outlet of the tower kettle reboiler of the circulating tower is connected with an inlet of the condenser at the top of the circulating tower, and a heat source outlet of the tower kettle reboiler of the concentrating tower is connected with an inlet of the condenser at the top of the concentrating tower;
the cold material flow outlet of the tower top condenser of the salt tower, the low-boiling tower and the high-boiling tower is connected with the inlet of a compressor B, the outlet of the compressor B is respectively connected with the tower kettle reboiler of the salt tower, the tower kettle reboiler of the low-boiling tower and the heat source inlet of the tower kettle reboiler of the high-boiling tower, the heat source outlet of the tower kettle reboiler of the salt tower is connected with the inlet of the tower top condenser of the salt tower, the heat source outlet of the tower kettle reboiler of the low-boiling tower is connected with the inlet of the tower top condenser of the low-boiling tower, and the heat source outlet of the tower kettle reboiler of the high-boiling tower is connected with the inlet of the tower top condenser of the high-boiling tower.
In the technical scheme, a flash tank A is arranged between a cold material flow inlet of a condenser at the top of the circulating tower and a heat source outlet of a reboiler at the bottom of the circulating tower, the heat source outlet of the reboiler at the bottom of the circulating tower is connected with a liquid inlet of the flash tank A, a liquid outlet of the flash tank A is connected with a cold material flow inlet of the condenser at the top of the circulating tower, and the flash tank A is provided with a flash steam outlet and is connected with an inlet of the compressor A;
a heat source outlet of a reboiler at the tower bottom of the concentrating tower is connected with a liquid inlet of the flash tank A, and a liquid outlet of the flash tank A is connected with a cold material flow inlet of a condenser at the top of the concentrating tower;
a flash tank B is arranged between the cold material flow inlet of the condenser at the top of the salt tower and the heat source outlet of the reboiler at the bottom of the salt tower, the heat source outlet of the reboiler at the bottom of the salt tower is connected with the liquid inlet of the flash tank B, the liquid outlet of the flash tank B is connected with the cold material flow inlet of the condenser at the top of the salt tower, and the flash tank B is provided with a flash steam outlet and is connected with the inlet of the compressor B;
a heat source outlet of the reboiler at the tower bottom of the low-boiling tower is connected with a liquid inlet of the flash tank B, and a liquid outlet of the flash tank B is connected with a cold material flow inlet of a condenser at the tower top of the low-boiling tower;
and a heat source outlet of the reboiler at the tower bottom of the high-boiling tower is connected with a liquid inlet of the flash tank B, and a liquid outlet of the flash tank B is connected with a cold material flow inlet of a condenser at the top of the high-boiling tower.
In the technical scheme, a circulating tower circulating pump is arranged on a connecting pipeline between a liquid outlet of the flash tank A and a cold material flow inlet of a condenser at the top of the circulating tower, a concentrating tower circulating pump is arranged on a connecting pipeline between a liquid outlet of the flash tank A and a cold material flow inlet of a condenser at the top of the concentrating tower, and a cold material flow circulating outlet is arranged on each of the condenser at the top of the circulating tower and the condenser at the top of the concentrating tower and is connected with a circulating inlet of the flash tank A;
the liquid outlet of flash drum B and the connecting pipeline of the cold commodity circulation entry of salt tower top condenser are equipped with a salt tower circulating pump, and the liquid outlet of flash drum B and the connecting pipeline of the cold commodity circulation entry of low boiling tower top condenser are equipped with a low boiling tower circulating pump, and the liquid outlet of flash drum B and the connecting pipeline of the cold commodity circulation entry of high boiling tower top condenser are equipped with a high boiling tower circulating pump, and salt tower top condenser, low boiling tower top condenser and high boiling tower top condenser all are equipped with a cold commodity circulation export and link to each other with the circulation import of flash drum B.
An energy-saving working method of a BDO rectifying device is characterized in that raw materials enter a catalytic reactor to react to obtain 1, 4-butynediol, water, a mixture of formaldehyde and methanol and are sent to a circulating tower for rectification, steam at the top of the circulating tower comprises formaldehyde, water and methanol, the steam at the top of the circulating tower enters a condenser at the top of the circulating tower and is condensed into tower top condensate, one part of the tower top condensate reflows to the top of the circulating tower, the other part of the tower top condensate is extracted, tower kettle extract liquid of the 1, 4-butynediol and water obtained at the tower kettle of the circulating tower enters a hydrogenation reactor for reaction, and the mixture of BDO, water and butanol enters a concentration tower for rectification;
steam at the top of the concentrating tower comprises water and butanol, the steam at the top of the concentrating tower enters a condenser at the top of the concentrating tower and is condensed into tower top condensate, one part of the tower top condensate reflows to the top of the concentrating tower, the other part of the tower top condensate is extracted, the extracted liquid at the bottom of the concentrating tower comprises BDO, and water and high-boiling-point substances are sent into the salt tower for rectification;
rectifying the salt tower to obtain salt tower top steam containing BDO, water and low-boiling-point substances, feeding the salt tower top steam into a salt tower top condenser, condensing the salt tower top steam into tower top condensate, refluxing one part of the tower top condensate to the top of the salt tower, feeding the other part of the tower top condensate into the low-boiling-point tower for rectification, and obtaining BDO and tar in a salt tower kettle;
after rectification, low-boiling tower top steam containing water, BDO and low-boiling residues enters a low-boiling tower top condenser to be condensed into tower top condensate, one part of the tower top condensate reflows to the tower top of the low-boiling tower, the other part of the tower top condensate is extracted, and BDO and high-boiling residues obtained in a tower kettle of the low-boiling tower are sent into a high-boiling tower to be continuously rectified;
rectifying to obtain high-boiling tower top steam containing BDO and water, feeding the high-boiling tower top steam into a high-boiling tower top condenser, condensing to obtain tower top condensate, refluxing one part of the tower top condensate to the top of a high-boiling tower, extracting the other part of the tower top condensate, extracting a BDO product from a side line of the high-boiling tower, and obtaining a mixture of BDO and high-boiling substances from a tower kettle of the high-boiling tower;
respectively feeding water into a condenser at the top of the circulating tower and a condenser at the top of the concentrating tower, partially gasifying the water into water vapor after absorbing heat, then feeding the water vapor into a compressor A for heating, feeding the heated water vapor into a reboiler at the bottom of the circulating tower and a reboiler at the bottom of the concentrating tower respectively for phase change and condensing the water vapor into saturated water, feeding the saturated water into a flash tank A for adiabatic flash evaporation to obtain flash vapor and condensate, feeding the flash vapor into the compressor A for recompression, feeding one part of the condensate back to the condenser at the top of the circulating tower through a circulating pump of the circulating tower, feeding the other part of the condensate back to the condenser at the top of the concentrating tower through a circulating pump of the concentrating tower, and feeding the liquid which is not gasified in the condenser at the top of the circulating tower and the condenser at the top of the concentrating tower back into the flash tank A;
water is respectively sent into the salt tower top condenser, the low-boiling tower top condenser and the high-boiling tower top condenser, the water is partially gasified into water vapor after absorbing heat and then enters the compressor B for heating, the heated water vapor respectively enters the salt tower kettle reboiler, the low-boiling tower kettle reboiler and the high-boiling tower kettle reboiler are subjected to phase change and condensed into saturated water, the saturated water enters a flash tank B to carry out adiabatic flash evaporation to obtain flash steam and condensate, the flash steam enters a compressor B to be compressed again, and part of the condensate returns to a condenser at the top of the salt tower through a salt tower circulating pump, part of the condensate returns to a condenser at the top of the low-boiling tower through a low-boiling tower circulating pump, and part of the condensate returns to a condenser at the top of the high-boiling tower through a high-boiling tower circulating pump, and the liquid which is not gasified in the condenser at the top of the salt tower, the condenser at the top of the low-boiling tower and the condenser at the top of the high-boiling tower flows back to the flash tank B.
In the technical scheme, the condenser at the top of the circulating tower, the condenser at the top of the concentrating tower, the condenser at the top of the salt tower, the condenser at the top of the low-boiling tower and the condenser at the top of the high-boiling tower are all in a horizontal tube falling film type, and the gasification rate of water is 0.1-0.4.
In the technical scheme, the top pressure of the circulating tower is 450-550 kPa, the temperature is 130-150 ℃, the top pressure of the concentrating tower is 165-175 kPa, the temperature is 100-120 ℃, the top pressure of the salt tower is 3-7 kPa, the temperature is 120-140 ℃, the top pressure of the low-boiling tower is 4-8 kPa, the temperature is 140-160 ℃, the top pressure of the high-boiling tower is 4-8 kPa, and the temperature is 140-160 ℃.
In the technical scheme, the number of theoretical plates of the circulating tower is 45-52, the reflux ratio is 0.5-0.7, the number of theoretical plates of the concentrating tower is 18-24, the reflux ratio is 0.1-0.2, the number of theoretical plates of the salt tower is 20-27, the reflux ratio is 0.2-0.3, the number of theoretical plates of the low-boiling tower is 26-32, the reflux ratio is 0.5-0.7, the number of theoretical plates of the high-boiling tower is 38-42, the side-line extraction amount is A, the tower top extraction amount is B, and the reflux ratio is A/(0.36B).
In the technical scheme, the pressure ratio of the compressor A to the compressor B is 3-5.
In the technical scheme, the concentration of BDO extracted from the tower kettle of the concentrating tower is more than or equal to 94 percent, and the concentration of BOD products extracted from the side line of the high-boiling tower is more than or equal to 99.7 percent.
The invention has the advantages and beneficial effects that:
1. according to the energy-saving BDO rectification device and method, the compressor is driven by clean electric energy to heat the steam at the top of the tower, a heat source is provided for the tower kettle, the use of a large amount of steam and circulating water is saved, and the operation cost can be saved by about 68.7% each year under the same working condition;
2. according to the energy-saving BDO rectification device and the method, the tower top condenser is in a horizontal pipe falling film type, hot materials pass through a pipe pass, cold materials pass through a shell pass, water (cold materials) in the flash tank is continuously conveyed into the tower top condenser through the tower top circulating pump, heat of condensation phase change of tower top steam is absorbed and evaporated, and the heat transfer efficiency of the condenser is greatly improved through the combined use of the horizontal pipe falling film type condenser and the circulating pump;
3. according to the energy-saving BDO rectification device and method, the flash tank is arranged, the heat-exchanged tower top condensate is subjected to adiabatic flash evaporation, the flashed steam returns to the inlet of the compressor to be compressed continuously, so that the heat recovery of the tower top steam is more sufficient, and the use of a large amount of cooling water is saved by a flash evaporation cooling mode.
Drawings
FIG. 1a is a flow chart of example 1 of the present invention;
fig. 1b is a flowchart of embodiment 1 of the present invention (continuing to fig. 1 a).
Wherein, 1 is a circulating tower, 2 is a circulating tower top condenser, 3 is a compressor A, 4 is a concentrating tower top condenser, 5 is a concentrating tower, 6 is a flash tank A, 7 is a salt tower, 8 is a salt tower top condenser, 9 is a low-boiling tower top condenser, 10 is a low-boiling tower, 11 is a high-boiling tower top condenser, 12 is a high-boiling tower, 13 is a flash tank B, 14 is a circulating pump of the circulating tower, 15 is a circulating pump of the concentrating tower, 16 is a circulating pump of the salt tower, 17 is a circulating pump of the low-boiling tower, 18 is a circulating pump of the high-boiling tower, 19 is a catalytic reactor, 20 is a hydrogenation reactor, and 21 is a compressor B.
Detailed Description
In order to make the technical solution of the present invention better understood, the technical solution of the present invention is further described below with reference to the accompanying drawings and specific embodiments.
Example 1
An energy-saving BDO rectifying device comprises a catalytic reactor 19, a circulating tower 1, a hydrogenation reactor 20, a concentration tower 5, a salt tower 7, a low-boiling tower 10 and a high-boiling tower 12, wherein an outlet of the catalytic reactor is connected with an inlet of the circulating tower, a tower bottom liquid outlet of the circulating tower is connected with an inlet of the hydrogenation reactor, an outlet of the hydrogenation reactor is connected with an inlet of the concentration tower, a tower bottom liquid outlet of the concentration tower is connected with an inlet of the salt tower, a material outlet of a tower top condenser of the salt tower is connected with a feed inlet of the low-boiling tower, a tower bottom liquid outlet of the low-boiling tower is connected with a feed inlet of the high-boiling tower, and a side draw outlet of the high-boiling tower is a BDO product outlet;
the circulating tower, the concentration tower, the salt tower, the low-boiling tower and the high-boiling tower are all provided with a horizontal tube falling film type tower top condenser and a tower kettle reboiler,
cold material flow outlets of the tower top condenser 2 of the circulating tower and the tower top condenser 4 of the concentration tower are connected with an inlet of a compressor A3, outlets of the compressor A are respectively connected with a tower kettle reboiler of the circulating tower and a heat source inlet of a tower kettle reboiler of the concentration tower, a heat source outlet of the tower kettle reboiler of the circulating tower is connected with an inlet of the tower top condenser of the circulating tower, and a heat source outlet of the tower kettle reboiler of the concentration tower is connected with an inlet of the tower top condenser of the concentration tower;
salt tower top condenser 8, the cold material stream export of low boiling tower top condenser 9 and high boiling tower top condenser 11 all links to each other with a compressor B21's entry, compressor B's export respectively with the tower cauldron reboiler of salt tower, the tower cauldron reboiler of low boiling tower and the heat source entry of the tower cauldron reboiler of high boiling tower link to each other, the heat source export of salt tower cauldron reboiler links to each other with the entry of salt tower top condenser, the heat source export of low boiling tower cauldron reboiler links to each other with the entry of low boiling tower top condenser, the heat source export of high boiling tower cauldron reboiler links to each other with the entry of high boiling tower top condenser.
A flash tank A6 is arranged between the cold material flow inlet of the condenser at the top of the circulating tower and the heat source outlet of the reboiler at the bottom of the circulating tower, the heat source outlet of the reboiler at the bottom of the circulating tower is connected with the liquid inlet of the flash tank A, the liquid outlet of the flash tank A is connected with the cold material flow inlet of the condenser at the top of the circulating tower, and the flash tank A is provided with a flash steam outlet and is connected with the inlet of the compressor A;
a heat source outlet of a reboiler at the tower bottom of the concentrating tower is connected with a liquid inlet of a flash tank A, and a liquid outlet of the flash tank A is connected with a cold material flow inlet of a condenser at the top of the concentrating tower;
a flash tank B13 is arranged between the cold material flow inlet of the condenser at the top of the salt tower and the heat source outlet of the reboiler at the bottom of the salt tower, the heat source outlet of the reboiler at the bottom of the salt tower is connected with the liquid inlet of a flash tank B13, the liquid outlet of the flash tank B is connected with the cold material flow inlet of the condenser at the top of the salt tower, and the flash tank B is provided with a flash steam outlet and is connected with the inlet of a compressor B;
a heat source outlet of a reboiler at the tower bottom of the low-boiling tower is connected with a liquid inlet of a flash tank B, and a liquid outlet of the flash tank B is connected with a cold material flow inlet of a condenser at the tower top of the low-boiling tower;
and a heat source outlet of a reboiler of the high-boiling tower is connected with a liquid inlet of the flash tank B, and a liquid outlet of the flash tank B is connected with a cold material flow inlet of a condenser at the top of the high-boiling tower.
A circulating tower circulating pump 14 is arranged on a connecting pipeline between the liquid outlet of the flash tank A and the cold material flow inlet of the condenser at the top of the circulating tower, a concentrating tower circulating pump 15 is arranged on a connecting pipeline between the liquid outlet of the flash tank A and the cold material flow inlet of the condenser at the top of the concentrating tower, and the condenser at the top of the circulating tower and the condenser at the top of the concentrating tower are both provided with a cold material flow circulating outlet connected with the circulating inlet of the flash tank A;
a salt tower circulating pump 16 is arranged on a connecting pipeline between the liquid outlet of the flash tank B and the cold material flow inlet of the condenser at the top of the salt tower, a low-boiling tower circulating pump 17 is arranged on a connecting pipeline between the liquid outlet of the flash tank B and the cold material flow inlet of the condenser at the top of the low-boiling tower, a high-boiling tower circulating pump 18 is arranged on a connecting pipeline between the liquid outlet of the flash tank B and the cold material flow inlet of the condenser at the top of the high-boiling tower, and the condenser at the top of the salt tower, the condenser at the top of the low-boiling tower and the condenser at the top of the high-boiling tower are all provided with a cold material flow circulating outlet connected with the circulating inlet of the flash tank B.
An energy-saving BDO rectifying device working method comprises the steps of adding raw materials into a catalytic reactor for reaction, feeding a mixture of 42t/h of 1, 4-butynediol 36.8%, water 48.9%, formaldehyde 9.8%, methanol 3.7%, propiolic alcohol 0.4%, sodium formate 0.3% and formic acid 0.1% into a circulating tower for rectification, wherein the tower top pressure of the circulating tower is 512kPa, the temperature is 146 ℃, the tower bottom temperature is 160 ℃, the reflux ratio is 0.6, and the number of theoretical plates is 50. The steam at the top of the circulating tower comprises 30.1 percent of formaldehyde, 57.3 percent of water, 11.6 percent of methanol, 0.8 percent of propiolic alcohol and 0.2 percent of formic acid, the steam at the top of the circulating tower enters a condenser at the top of the circulating tower and is condensed into a condensed liquid at the top of the circulating tower, one part of the condensed liquid at the top of the circulating tower reflows to the top of the circulating tower, the other part of the condensed liquid is extracted, the extracted amount is 12.2t/h, 53.8 percent of 1, 4-butynediol, 45.1 percent of water, 0.4 percent of formaldehyde, 0.4 percent of sodium formate, 0.2 percent of propiolic alcohol and 0.1 percent of formic acid are obtained at the bottom of the circulating tower, the extracted liquid is filtered by a fine filtration system to remove a catalyst and then enters a hydrogenation reactor for reaction, and a mixture of BDO 54 percent, water 43.5 percent, butanol 1.0 percent of butanol, 0.6 percent of high-boiling substance, 0.5 percent of sodium formate and 0.3 percent of methanol is distilled at 27.8t/h and enters a concentration tower for rectification;
the pressure of the top of the concentrating tower is 169kPa, the temperature is 111 ℃, the temperature of the bottom of the tower is 163 ℃, the reflux ratio is 0.15, the number of theoretical plates is 21, the steam at the top of the concentrating tower comprises 96.9 percent of water, 2.2 percent of butanol, 0.6 percent of methanol and 0.2 percent of propanol, the steam at the top of the concentrating tower enters a condenser at the top of the concentrating tower and is condensed into a condensate at the top of the tower, one part of the condensate at the top of the tower reflows to the top of the concentrating tower, the other part of the condensate is taken as extraction at 11.6t/h, and the extract at the bottom of the concentrating tower comprises 16.1t/h of BDO 94 percent, 4.9 percent of water, 1.0 percent of high-boiling substances and 0.8 percent of sodium formate and is sent to a salt tower for rectification;
the pressure of the top of the salt tower is 5.2kPa, the temperature is 135 ℃, the temperature of the bottom of the tower is 161 ℃, the number of theoretical plates is 25, the reflux ratio is 0.25, steam at the top of the salt tower for rectifying to obtain BDO 94%, water is 5.0%, low-boiling-point substances are 0.6% and high-boiling-point substances are 0.1% enters a condenser at the top of the salt tower and is condensed to top condensate, one part of the top condensate reflows to the top of the salt tower, the other part of the top condensate is sent to the low-boiling-point tower for rectifying, and BDO85% and tar 15% are obtained at the bottom of the salt tower;
the top pressure of the low-boiling tower is 6.3kPa, the temperature is 150 ℃, the temperature of the tower kettle is 162 ℃, the reflux ratio is 0.6, the number of theoretical plates is 30, the steam at the top of the low-boiling tower containing 20.4 percent of BDO, 68.4 percent of water and 8.4 percent of low-boiling substances enters a condenser at the top of the low-boiling tower after rectification to be condensed into tower top condensate, one part of the tower top condensate reflows to the top of the low-boiling tower, the other part of the tower top condensate is extracted, the extraction amount is 1085kg/h, 99.5 percent of BDO and 0.4 percent of high-boiling substances obtained at the tower kettle of the low-boiling tower are sent into a high-boiling tower for continuous rectification;
the pressure of the top of the high-boiling tower is 6.3kPa, the temperature is 150 ℃, the temperature of a tower kettle is 166 ℃, the number of theoretical plates is 40, the reflux ratio is 275, steam at the top of the high-boiling tower with 99.2 percent of BDO and 0.7 percent of water obtained by rectification enters a condenser at the top of the high-boiling tower and is condensed into tower top condensate, one part of the tower top condensate reflows to the top of the high-boiling tower, the other part of the tower top condensate is extracted, the extraction amount is 138kg/h, 13659kg/h of BDO product with the concentration of 99.8 percent is obtained by side extraction of the high-boiling tower, and the product purity requirement is met. A mixture of 85.6 percent of BDO and 10.2 percent of high-boiling-point substances is obtained at the tower bottom of the high-boiling tower;
feeding 19.3t/h of water into a condenser at the top of a circulating tower, feeding 5.8t/h of water into a condenser at the top of a concentration tower, after absorbing heat, partially gasifying the water into steam, then feeding the steam into a compressor A to increase the temperature to 170 ℃, wherein the pressure is 700kPa, feeding the steam after temperature rise into a reboiler at the bottom of the circulating tower and a reboiler at the bottom of the concentration tower respectively to carry out phase change and condense the steam into saturated water, feeding the saturated water into a flash tank A to carry out adiabatic flash evaporation to obtain flash steam and condensate, feeding the flash steam into the compressor A to carry out recompression, feeding one part of the condensate back to the condenser at the top of the circulating tower through a circulating pump of the circulating tower, and feeding the other part of the condensate back to the condenser at the top of the circulating towerReturning to the condenser at the top of the concentrating tower through a circulating pump of the concentrating tower, wherein the gasification rates of the condenser at the top of the circulating tower and the condenser at the top of the concentrating tower are 0.3, the liquid which is not gasified flows back to the flash tank A, and the circulating amount of the circulating pump of the circulating tower is 400m3Per hour, the circulation flow of the circulating pump of the concentration tower is 200m3/h;
Feeding 5.4t/h of water into a condenser at the top of a salt tower, feeding 3.4t/h of water into a condenser at the top of a low-boiling tower, feeding 14t/h of water into a condenser at the top of a high-boiling tower, absorbing heat, gasifying the water into water vapor, then feeding the water vapor into a compressor B, heating the water vapor to 174 ℃, wherein the pressure is 770kPa, the water vapor after heating respectively enters a reboiler at the bottom of the salt tower, the reboiler at the bottom of the low-boiling tower and the reboiler at the bottom of the high-boiling tower are subjected to phase change and condensed into saturated water, the saturated water enters a flash tank B and is subjected to adiabatic flash evaporation to obtain flash vapor and condensate, the flash vapor enters the compressor B to be compressed again, one part of the condensate returns to the condenser at the top of the salt tower through a circulating pump of the salt tower, one part returns to the condenser at the top of the low-boiling tower through a circulating pump of the low-boiling tower, one part returns to the condenser at the top of the high-boiling tower through a circulating pump, the condenser at the top of the salt tower, the condenser at the top of the low-boiling tower and the high-boiling tower, the condenser at the top of the salt tower, the high-boiling tower, the condenser at the gasification rate of 0.3, the liquid which is not gasified flows back to the flash tank B, and the circulation amount of the circulating pump of the salt tower is 100m3Per hour, the circulation amount of the circulating pump of the low-boiling tower is 100m3Per hour, the circulation amount of the circulating pump of the low-boiling tower is 200m3/h。
The heat at the top of the tower is recycled and used for the tower kettle, and each rectifying tower can meet the operation requirement only by supplementing a small amount of steam or even without additionally supplementing steam. Wherein the circulating tower needs to supplement steam for 20t/h, the concentration tower needs to supplement steam for 1.5t/h, the salt tower needs to supplement steam for 1.5t/h, the low-boiling tower needs to supplement steam for 3.2t/h, and the high-boiling tower does not need to supplement steam. The power of compressor A was 4550kW, and the power of compressor B was 2240 kW.
In this embodiment, water and the overhead steam heat transfer recovery heat back gasification reach the temperature that matches with the tower cauldron for vapor through the heating of compressor again, then condense in the reboiler and bring the heat to the tower cauldron, and the continuous phase transition that takes place of this process water. Water is used as an intermediate medium, so that substances such as formic acid in the overhead steam are prevented from entering a compressor. In this technical scheme, water takes place the phase transition as the intermediate medium and material heat transfer, heat transfer coefficient is higher than the heat transfer process that does not have the phase transition, horizontal pipe falling liquid film condenser's rate of gasification is controlled at 0.1~0.4, be more favorable to water to form a film on the pipe wall, combine the use of circulating pump simultaneously, the heat transfer process has further been reinforceed, the loss of the difference in temperature of heat transfer in this process is less, make the export steam temperature of compressor and the difference in temperature of tower bottom liquid can 6~8 ℃, avoided the compressor to consume more power and improve the temperature of export steam.
In the embodiment, the steam condensate flowing out of the tower top condenser is subjected to adiabatic flash evaporation, and the flashed steam returns to the inlet of the compressor to be compressed continuously, so that the heat recovery of the tower top steam is more sufficient, and the use of circulating cooling water is saved.
Example 2
In this embodiment, the arrangement of the reaction and rectification apparatus, i.e., the catalytic reactor, the circulation tower, the hydrogenation reactor, the concentration tower, the salt tower, the low-boiling tower and the high-boiling tower, is the same as that in embodiment 1, except that in embodiment 1, the circulation tower and the concentration tower share one compressor and one flash tank, and the salt tower, the low-boiling tower and the high-boiling tower share one compressor and one flash tank. When the handling capacity is larger, the multiple rectifying towers share the compressor, so that the shaft power is overlarge, and the selection of the compressor is limited, therefore, the device is suitable for the working condition with larger handling capacity.
Comparative example 1
In this comparative example, the throughput and operating parameters of all the rectification columns were the same as in example 1, except that no overhead heat recovery unit, i.e., no compressor, flash tank and circulating pump, was provided. The steam consumption of the circulating tower, the concentration tower, the salt tower, the low-boiling tower and the high-boiling tower are respectively44t/h, 18t/h, 9t/h, 8t/h and 17t/h, and the amount of circulating water consumed by the overhead condenser is 2100 m respectively3/h,980 m3/h,450 m3/h,400 m3/h ,1000m3/h。
This comparative example compares the operating costs with example 1: (according to the specific situation of the location of the device, the price of steam is 180 yuan/ton, the price of electricity is 0.65 yuan/degree, and the price of cooling water is 0.2 yuan/m3Running every year 8000 hours for calculation)
Figure 818155DEST_PATH_IMAGE001
Through calculation, compared with the prior art, the energy-saving rectifying device and the method can save about 68.7 percent of production operation cost and greatly save the production cost. The method is more competitive in areas with the shortage of steam and higher steam price.
The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.

Claims (9)

1. An energy-saving BDO rectifying device is characterized by comprising a catalytic reactor, a circulating tower, a hydrogenation reactor, a concentration tower, a salt tower, a low-boiling tower and a high-boiling tower, wherein an outlet of the catalytic reactor is connected with an inlet of the circulating tower, a tower bottom liquid outlet of the circulating tower is connected with an inlet of the hydrogenation reactor, an outlet of the hydrogenation reactor is connected with an inlet of the concentration tower, a tower bottom liquid outlet of the concentration tower is connected with an inlet of the salt tower, a material outlet of a tower top condenser of the salt tower is connected with a feed inlet of the low-boiling tower, a tower bottom liquid outlet of the low-boiling tower is connected with a feed inlet of the high-boiling tower, and a side draw outlet of the high-boiling tower is a product outlet of BDO;
the circulating tower, the concentration tower, the salt tower, the low-boiling tower and the high-boiling tower are all provided with a tower top condenser and a tower kettle reboiler,
cold material flow outlets of the condenser at the top of the circulating tower and the condenser at the top of the concentrating tower are both connected with an inlet of a compressor A, outlets of the compressor A are respectively connected with a tower kettle reboiler of the circulating tower and a heat source inlet of a tower kettle reboiler of the concentrating tower, a heat source outlet of the tower kettle reboiler of the circulating tower is connected with an inlet of the condenser at the top of the circulating tower, and a heat source outlet of the tower kettle reboiler of the concentrating tower is connected with an inlet of the condenser at the top of the concentrating tower;
the cold material flow outlet of the salt tower top condenser, the low-boiling tower top condenser and the high-boiling tower top condenser is connected with the inlet of a compressor B, the outlet of the compressor B is respectively connected with the tower kettle reboiler of the salt tower, the tower kettle reboiler of the low-boiling tower and the heat source inlet of the tower kettle reboiler of the high-boiling tower, the heat source outlet of the salt tower kettle reboiler is connected with the inlet of the salt tower top condenser, the heat source outlet of the low-boiling tower kettle reboiler is connected with the inlet of the low-boiling tower top condenser, and the heat source outlet of the high-boiling tower kettle reboiler is connected with the inlet of the high-boiling tower top condenser.
2. The energy-saving BDO rectification device according to claim 1, wherein a flash tank A is arranged between the condenser cold material flow inlet at the top of the circulating tower and the reboiler heat source outlet at the bottom of the circulating tower, the reboiler heat source outlet at the bottom of the circulating tower is connected with the liquid inlet of the flash tank A, the liquid outlet of the flash tank A is connected with the condenser cold material flow inlet at the top of the circulating tower, the flash tank A is provided with a flash steam outlet and is connected with the inlet of the compressor A;
a heat source outlet of a reboiler at the tower bottom of the concentrating tower is connected with a liquid inlet of the flash tank A, and a liquid outlet of the flash tank A is connected with a cold material flow inlet of a condenser at the top of the concentrating tower;
a flash tank B is arranged between the cold material flow inlet of the condenser at the top of the salt tower and the heat source outlet of the reboiler at the bottom of the salt tower, the heat source outlet of the reboiler at the bottom of the salt tower is connected with the liquid inlet of the flash tank B, the liquid outlet of the flash tank B is connected with the cold material flow inlet of the condenser at the top of the salt tower, and the flash tank B is provided with a flash steam outlet and is connected with the inlet of the compressor B;
a heat source outlet of the reboiler at the tower bottom of the low-boiling tower is connected with a liquid inlet of the flash tank B, and a liquid outlet of the flash tank B is connected with a cold material flow inlet of a condenser at the tower top of the low-boiling tower;
and a heat source outlet of the reboiler at the tower bottom of the high-boiling tower is connected with a liquid inlet of the flash tank B, and a liquid outlet of the flash tank B is connected with a cold material flow inlet of a condenser at the top of the high-boiling tower.
3. The energy-saving BDO rectification device as claimed in claim 2, wherein a circulating tower circulating pump is arranged on a connecting pipeline between the liquid outlet of the flash tank A and the cold material flow inlet of the condenser at the top of the circulating tower, a concentrating tower circulating pump is arranged on a connecting pipeline between the liquid outlet of the flash tank A and the cold material flow inlet of the condenser at the top of the concentrating tower, and the condenser at the top of the circulating tower and the condenser at the top of the concentrating tower are respectively provided with a cold material flow circulating outlet connected with the circulating inlet of the flash tank A;
the liquid outlet of flash drum B and the connecting pipeline of the cold commodity circulation entry of salt tower top condenser are equipped with a salt tower circulating pump, and the liquid outlet of flash drum B and the connecting pipeline of the cold commodity circulation entry of low boiling tower top condenser are equipped with a low boiling tower circulating pump, and the liquid outlet of flash drum B and the connecting pipeline of the cold commodity circulation entry of high boiling tower top condenser are equipped with a high boiling tower circulating pump, and salt tower top condenser, low boiling tower top condenser and high boiling tower top condenser all are equipped with a cold commodity circulation export and link to each other with the circulation import of flash drum B.
4. The working method of the energy-saving BDO rectification device as claimed in claim 3, wherein the raw material enters the catalytic reactor to react to obtain 1, 4-butynediol, the mixture of water, formaldehyde and methanol is sent to the circulating tower to be rectified, the vapor at the top of the circulating tower comprises formaldehyde, water and methanol, the vapor at the top of the circulating tower enters the condenser at the top of the circulating tower to be condensed into a tower top condensate, one part of the tower top condensate flows back to the top of the circulating tower, the other part of the tower top condensate is extracted, the tower bottom extract of the circulating tower, which obtains 1, 4-butynediol and water, enters the hydrogenation reactor to react to obtain BDO, and the mixture of water and butanol enters the concentrating tower to be rectified;
steam at the top of the concentrating tower comprises water and butanol, the steam at the top of the concentrating tower enters a condenser at the top of the concentrating tower and is condensed into tower top condensate, one part of the tower top condensate reflows to the top of the concentrating tower, the other part of the tower top condensate is extracted, the extracted liquid at the bottom of the concentrating tower comprises BDO, and water and high-boiling-point substances are sent into the salt tower for rectification;
rectifying the salt tower to obtain salt tower top steam containing BDO, water and low-boiling-point substances, feeding the salt tower top steam into a salt tower top condenser, condensing the salt tower top steam into tower top condensate, refluxing one part of the tower top condensate to the top of the salt tower, feeding the other part of the tower top condensate into the low-boiling-point tower for rectification, and obtaining BDO and tar in a salt tower kettle;
after rectification, low-boiling tower top steam containing water, BDO and low-boiling residues enters a low-boiling tower top condenser to be condensed into tower top condensate, one part of the tower top condensate reflows to the tower top of the low-boiling tower, the other part of the tower top condensate is extracted, and BDO and high-boiling residues obtained in a tower kettle of the low-boiling tower are sent into a high-boiling tower to be continuously rectified;
rectifying to obtain high-boiling tower top steam containing BDO and water, feeding the high-boiling tower top steam into a high-boiling tower top condenser, condensing to obtain tower top condensate, refluxing one part of the tower top condensate to the top of a high-boiling tower, extracting the other part of the tower top condensate, extracting a BDO product from a side line of the high-boiling tower, and obtaining a mixture of BDO and high-boiling substances from a tower kettle of the high-boiling tower;
respectively feeding water into a condenser at the top of the circulating tower and a condenser at the top of the concentrating tower, partially gasifying the water into water vapor after absorbing heat, then feeding the water vapor into a compressor A for heating, feeding the heated water vapor into a reboiler at the bottom of the circulating tower and a reboiler at the bottom of the concentrating tower respectively for phase change and condensing the water vapor into saturated water, feeding the saturated water into a flash tank A for adiabatic flash evaporation to obtain flash vapor and condensate, feeding the flash vapor into the compressor A for recompression, feeding one part of the condensate back to the condenser at the top of the circulating tower through a circulating pump of the circulating tower, feeding the other part of the condensate back to the condenser at the top of the concentrating tower through a circulating pump of the concentrating tower, and feeding the liquid which is not gasified in the condenser at the top of the circulating tower and the condenser at the top of the concentrating tower back into the flash tank A;
water is respectively sent into the salt tower top condenser, the low-boiling tower top condenser and the high-boiling tower top condenser, the water is partially gasified into water vapor after absorbing heat and then enters the compressor B for heating, the heated water vapor respectively enters the salt tower kettle reboiler, the low-boiling tower kettle reboiler and the high-boiling tower kettle reboiler are subjected to phase change and condensed into saturated water, the saturated water enters a flash tank B to carry out adiabatic flash evaporation to obtain flash steam and condensate, the flash steam enters a compressor B to be compressed again, and part of the condensate returns to a condenser at the top of the salt tower through a salt tower circulating pump, part of the condensate returns to a condenser at the top of the low-boiling tower through a low-boiling tower circulating pump, and part of the condensate returns to a condenser at the top of the high-boiling tower through a high-boiling tower circulating pump, and the liquid which is not gasified in the condenser at the top of the salt tower, the condenser at the top of the low-boiling tower and the condenser at the top of the high-boiling tower flows back to the flash tank B.
5. The working method of the energy-saving BDO rectification device as claimed in claim 4, wherein the condenser at the top of the circulating tower, the condenser at the top of the concentrating tower, the condenser at the top of the salt tower, the condenser at the top of the low-boiling tower and the condenser at the top of the high-boiling tower are all in a horizontal tube falling film type, and the gasification rate of water is 0.1-0.4.
6. The working method of the energy-saving BDO rectification device according to claim 5, characterized in that the tower top pressure of the circulating tower is 450-550 kPa, the temperature is 130-150 ℃, the tower top pressure of the concentrating tower is 165-175 kPa, the temperature is 100-120 ℃, the tower top pressure of the salt tower is 3-7 kPa, the temperature is 120-140 ℃, the tower top pressure of the low-boiling tower is 4-8 kPa, the temperature is 140-160 ℃, the tower top pressure of the high-boiling tower is 4-8 kPa, and the temperature is 140-160 ℃.
7. The working method of the energy-saving BDO rectification device as claimed in claim 6, wherein the theoretical plate number of the circulating tower is 45-52, the reflux ratio is 0.5-0.7, the theoretical plate number of the concentrating tower is 18-24, the reflux ratio is 0.1-0.2, the theoretical plate number of the salt tower is 20-27, the reflux ratio is 0.2-0.3, the theoretical plate number of the low-boiling tower is 26-32, the reflux ratio is 0.5-0.7, the theoretical plate number of the high-boiling tower is 38-42, the side-draw amount is A, the overhead draw amount is B, and the reflux ratio is A/(0.36B).
8. The working method of the energy-saving BDO rectification device as claimed in claim 7, wherein the pressure ratio of the compressor A to the compressor B is 3-5.
9. The working method of the energy-saving BDO rectification device as claimed in claim 8, wherein the concentration of BDO extracted from the bottom of the concentrating tower is more than or equal to 94 percent, and the concentration of BOD products extracted from the side line of the high boiling tower is more than or equal to 99.7 percent.
CN202111184505.4A 2021-10-12 2021-10-12 Energy-saving BDO (BDO) rectifying device and method Pending CN113617050A (en)

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