CN115245791B - Device and method for producing alpha-alkyl ester of high-end fine chemicals - Google Patents
Device and method for producing alpha-alkyl ester of high-end fine chemicals Download PDFInfo
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- CN115245791B CN115245791B CN202210987659.5A CN202210987659A CN115245791B CN 115245791 B CN115245791 B CN 115245791B CN 202210987659 A CN202210987659 A CN 202210987659A CN 115245791 B CN115245791 B CN 115245791B
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- 239000012847 fine chemical Substances 0.000 title claims description 16
- 238000004519 manufacturing process Methods 0.000 title description 8
- 239000002994 raw material Substances 0.000 claims abstract description 153
- 239000007788 liquid Substances 0.000 claims abstract description 88
- 150000002148 esters Chemical class 0.000 claims abstract description 80
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 claims abstract description 62
- 239000003054 catalyst Substances 0.000 claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 48
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 35
- 239000001257 hydrogen Substances 0.000 claims description 32
- 229910052739 hydrogen Inorganic materials 0.000 claims description 32
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 22
- 239000007789 gas Substances 0.000 claims description 15
- 239000000047 product Substances 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- 230000001105 regulatory effect Effects 0.000 claims description 11
- 239000002904 solvent Substances 0.000 claims description 10
- 238000010926 purge Methods 0.000 claims description 9
- 238000004062 sedimentation Methods 0.000 claims description 7
- 230000008021 deposition Effects 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000011084 recovery Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 239000012752 auxiliary agent Substances 0.000 claims description 3
- 238000007664 blowing Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 239000011343 solid material Substances 0.000 claims description 3
- 239000012265 solid product Substances 0.000 claims description 3
- 238000005728 strengthening Methods 0.000 claims description 3
- 238000005194 fractionation Methods 0.000 claims description 2
- 230000001737 promoting effect Effects 0.000 claims description 2
- 238000000926 separation method Methods 0.000 abstract description 3
- 238000001816 cooling Methods 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 description 7
- 238000010924 continuous production Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 125000005907 alkyl ester group Chemical group 0.000 description 2
- 230000003321 amplification Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000003199 nucleic acid amplification method Methods 0.000 description 2
- 239000008247 solid mixture Substances 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 239000011344 liquid material Substances 0.000 description 1
- UKVIEHSSVKSQBA-UHFFFAOYSA-N methane;palladium Chemical compound C.[Pd] UKVIEHSSVKSQBA-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/10—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The device comprises an ester raw material tank and an aldehyde raw material tank, wherein a variable frequency stirrer is arranged at the top of the ester raw material tank, the bottom of the ester raw material tank is connected with an ester raw material circulating pump, an inlet of the ester raw material feeding pump is connected with an ester raw material circulating pump outlet line, an outlet of the aldehyde raw material tank is connected with an aldehyde raw material feeding pump inlet, an inlet end of a pre-reactor is connected with an ester raw material feeding pump outlet line, an outlet of the pre-reactor is connected with an inlet end of the reactor, an inlet end of a gas-liquid cooling separator is connected with an outlet of the reactor, the top of the gas-liquid separator is connected with a gas discharge, the bottom of the gas-liquid separator is connected with a liquid level control valve, liquid is fed to a rectifying tower through the liquid level control valve, the bottom of the rectifying tower is connected with a catalyst separation inlet end, an outlet of the catalyst separator is connected with an inlet of the rectifying tower circulating pump, and an outlet of the rectifying tower circulating pump is connected with a heating kettle of the rectifying tower to form circulation. The invention has the characteristics of mild reaction conditions, short process flow and high product purity.
Description
Technical Field
The invention relates to the technical field of production of alpha-alkyl esters of high-end fine chemicals, in particular to a device and a method for producing the alpha-alkyl esters of the high-end fine chemicals.
Background
In the technical field of high-end fine chemical alpha-alkyl ester production, an intermittently operated reaction kettle is adopted, esters and aldehydes are used as raw materials, micron-sized palladium-carbon is used as a catalyst, and the reaction is carried out at the reaction temperature of 65 ℃ under the reaction pressure of 2MPa for 6-8 hours and in the hydrogen atmosphere to generate the high-end fine chemical alpha-alkyl ester with high added value, so that the high-end fine chemical alpha-alkyl ester has the advantages of long reaction time, poor mass and heat transfer efficiency, high manual operation cost, low automation degree, difficulty in realizing continuous production and adverse effect on post-scale amplification and industrial mass production.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a device and a method for producing high-end fine chemical alpha-alkyl ester, which have the characteristics of mild reaction conditions, short process flow and high product purity.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the device for producing the high-end fine chemicals alpha-alkyl ester comprises an ester raw material tank 1 and an aldehyde raw material tank 2, wherein a variable frequency stirrer is arranged at the top of the ester raw material tank 1, the bottom of the ester raw material tank is connected with an ester raw material circulating pump 3 to form a large amount of circulating raw materials, the variable frequency stirrer is arranged at the bottom of the aldehyde raw material tank 2, an inlet of the ester raw material feeding pump 4 is connected with an outlet pipeline of the ester raw material circulating pump 3, an outlet of the ester raw material feeding pump 4 is an ester raw material feeding flowmeter 6, an outlet of the aldehyde raw material tank 2 is connected with an inlet of the aldehyde raw material feeding pump 5 by adjusting the stroke and the variable frequency of the aldehyde raw material feeding pump 5, an inlet end of a pre-reactor 8 is connected with an outlet pipeline of the aldehyde raw material feeding pump 5, an outlet of the pre-reactor 8 is connected with an inlet end of a reactor 9, an inlet end of a gas-liquid cooling gas-liquid separator 10 is connected with an outlet of the reactor 9, a gas discharge valve 11 is connected with the top of the gas-liquid separator 10, a liquid level controller 12 is connected with a liquid level controller 12 and a liquid level controller 12 is connected with a liquid level controller 13 of the reactor 14, and a rectifying tower 13 is connected with a liquid level controller 13, and a rectifying tower is connected with a rectifying tower 13, and a rectifying tower 15 is connected with the bottom of the rectifying tower 13.
The bottom of the reactor 9 is provided with a stirrer for preventing a great deal of catalyst from sedimentation and deposition, further strengthening the mixing of the solvent and the raw materials, keeping the catalyst homogeneous, and enabling the hydrogen gas inlet at the bottom of the reactor 9 to enter in a micropore injection mode, enhancing micro-reaction and driving the catalyst to push to the top of the reactor 9.
The reactor 9 is a tubular reactor, and a temperature measuring device is arranged in the reactor, and can measure temperature of a plurality of sections of points of a central tube or can measure temperature of a side tube in an inserting manner; the top and the bottom of the reactor are all flange connection and sealing, a stirrer, a feed inlet and an air inlet are arranged on the flange at the bottom, the flange at the top of the reactor is provided with the air inlet and a material outlet, and a heating device and a heat preservation device are arranged outside the reactor.
The gas-liquid separator 10 is provided with a sedimentation pipe, the reacted product conveys the gas-liquid-solid mixture to the lower part of the gas-liquid separator 10, the gas is discharged to a gas recovery system from the top through a gas discharge valve 11 after being separated, and the liquid-solid material at the bottom of the separator is sent to a rectifying tower through a liquid level control valve 12 for fractionation; the gas-liquid separator 10 is provided with a heat preservation and heating system, a small amount of hydrogen entering from the bottom of the reaction condition can prevent catalyst deposition, and can promote unreacted substances in the product to further react completely, and the top of the separator is provided with a radar level gauge to form an automatic control system with a liquid level control valve of the separator.
The liquid-solid product separated by the gas-liquid separator 10 is sent to the bottom of the rectifying tower 13 through a separator liquid level control valve 12, and is heated to a certain temperature through a heater at the bottom of the rectifying tower 13, and alkyl ester and ethanol are separated in different tower layers respectively. A part of the product at the bottom of the rectifying tower flows out from the bottom to a catalyst separation system 14 together with the catalyst, and the separated liquid is circulated to the bottom of the rectifying tower 13 by a bottom rectifying tower circulating pump 15.
A method for using a device for producing high-end fine chemical alpha-alkyl ester, which comprises the following steps;
(1) And (3) blowing process gas: the method comprises the steps of filling nitrogen into the top of an ester raw material tank 1 and an aldehyde raw material tank 2, purging the raw material tank and a pump pipeline, adding a temporary pipeline, respectively purging a pre-reactor 8, a reactor 9 and a gas-liquid separator 10 with 1Mpa nitrogen, and purging a rectification system with 0.3Mpa nitrogen;
(2) And (3) cleaning a system: adding 50% of ethanol liquid level into an ester raw material tank 1 and an aldehyde raw material tank 2, starting a stirrer, starting an ester raw material circulating pump 3, an ester raw material feeding pump 4 and an aldehyde raw material feeding pump 5, enabling the feeding ratio to be 1:1, enabling the ethanol to be full of the ethanol, a reactor 8 and a reactor 9, enabling the liquid level of a separator to be 50% to discharge liquid, adding the ethanol into a rectifying tower to establish 50% liquid level, heating to 110 ℃, washing the rectifying tower, and circularly cleaning the ethanol of the whole system, wherein the detected impurity content is less than or equal to 0.5% and the system is cleaned;
(3) Initializing a device: the catalyst in the ester raw material tank 1 and the auxiliary agent are mixed according to a proportion and added into the raw material to 60%, and the ester raw material circulating pump 3 starts circulation; adding raw materials to 60% by weight of the aldehyde raw material tank 2, and starting a raw material tank stirrer; starting a hydrogen system after the airtight of the system is finished, starting the hydrogen system until the purity of the hydrogen reaches 99.9%, adjusting the CO content to be less than or equal to 10ppm, regulating the hydrogen amount of each path, ensuring that the pressure condition of the system under 2Mpa and the emptying system are in a stable state, pre-reacting the reactor 8, heating the reactor 9 to 65-90 ℃, pre-reacting the reactor 8, and starting a stirrer of the reactor 9; the separator liquid level was set to 30%; the liquid level of the rectifying tower 13 is established at 45-50%, the temperature is 60-80 ℃, and bottom circulation is established;
(4) The device starts: starting an ester raw material feeding pump 4, an aldehyde raw material feeding pump 5, and a ratio of the aldehyde raw material to the ester raw material being 4:6, feeding the system, keeping the liquid level of a separator to 35%, keeping the liquid level of a rectifying tower to be 45% -50%, gradually heating to 230 ℃ -260 ℃, and separating ethanol and alpha-alkyl ester from the rectifying tower 13;
(5) The device parks: the system is cooled to normal temperature, the system is depressurized to normal pressure, the ester raw material feed pump 4, the aldehyde raw material feed pump 5 and the ester raw material circulating pump 3 are started to circulate, residual raw materials of the ester raw material tank 1 and the aldehyde raw material tank 2 are discharged from a liquid outlet, products of the pre-reactor 8 and the reactor 9 are discharged, materials of the gas-liquid separator 10 and the rectifying tower 13 are discharged, the system is purged and replaced, and the stopping is finished.
The invention has the beneficial effects that:
1 the invention adopts a continuous production process to replace the traditional reaction kettle mode of intermittent operation, and overcomes the defects of long reaction time, poor mass and heat transfer efficiency, high manual operation cost, low automation degree, difficulty in realizing continuous production and inconvenience for subsequent large-scale amplification and industrialized mass production.
The continuous production method has the advantages of mild reaction conditions, short process flow, reliable operation, high safety, high economic benefit, large profit margin and the like, and can produce products with purity higher than 98 percent.
3. The ester raw material tank provided by the invention adopts a mixing mode of circulating and stirring to mix materials, so that the catalyst is ensured to be homogeneous and not easy to settle, and the problem that the catalyst is easy to settle in low-viscosity liquid materials is solved.
4. The invention adopts the pre-reactor, the materials react in advance, the load of the reactor is reduced, the reaction time of the materials in the reactor is shortened, the total reaction time of the materials is increased, and the reaction efficiency and the reaction effect are improved.
5. The pre-reactor, the reactor and the gas-liquid separator of the invention have hydrogen at the bottom and a heat preservation device, which is equivalent to lengthening the reaction time, promoting the complete reaction of materials and improving the conversion rate of materials.
6. The top of the pre-reactor and the bottom of the reactor are both provided with stirring and hydrogen entering from the bottom, so that the catalyst is ensured to be uniformly mixed in the materials, and the reaction is promoted.
7. The reaction temperature is 65 ℃, the reaction pressure is 2MPa, the reaction condition is mild, all raw materials of ester and aldehyde are converted into target products under the reaction condition, and the used solvent ethanol enters the reaction products and is recovered by a solvent recovery method, so that the solvent can be continuously used as a solvent.
Drawings
FIG. 1 is a schematic diagram of the structure of the present invention.
Reference numerals:
an ester raw material tank 1, an aldehyde raw material tank 2, an ester raw material circulating pump 3, an ester raw material feed pump 4, an aldehyde raw material feed pump 5, an ester raw material feed flow meter 6, an aldehyde raw material feed flow meter 7, a pre-reactor 8, a reactor 9, a gas-liquid separator 10, a gas discharge valve 11, a pressure reducing discharge valve 12, a rectifying column 13, a catalyst separator 14, a rectifying column circulating pump 15, ethanol 16, aldehyde 17, and alpha-alkyl ester 18.
Detailed Description
The present invention will be described in further detail with reference to examples.
As shown in fig. 1, the top of the ester raw material tank 1 is provided with a variable frequency stirrer, the bottom of the ester raw material tank 1 is connected with the ester raw material circulating pump 3 to form a large amount of circulating raw materials, so that the catalyst with the ratio of 1 ester to solvent ethanol of 1:1.3 and 0.1% (raw material aldehyde) is ensured to be uniformly mixed, and the catalyst is prevented from settling or gathering at the bottom of the ester raw material tank 1. The mixing ratio of aldehyde to solvent ethanol in the aldehyde raw material tank 2 is 1:1, and the two liquid miscible substances are mixed, so that the aldehyde raw material tank is uniformly stirred in advance only by a variable frequency stirrer arranged at the bottom of the aldehyde raw material tank, the ester raw material tank 1 is provided, and 0.3Mpa nitrogen is respectively arranged at the top of the aldehyde raw material tank 2 and is used for sealing and storing the nitrogen on one hand, and on the other hand, pressure is provided for a pump inlet.
The outlet of the ester raw material feeding pump 4 is an ester raw material feeding flowmeter 6, the feeding amount of the ester is regulated by regulating the stroke and the frequency conversion of the ester raw material feeding pump, the outlet of the aldehyde raw material feeding pump 5 is an aldehyde raw material feeding flowmeter 7, and the feeding amount of the aldehyde is regulated by regulating the stroke and the frequency conversion of the aldehyde raw material feeding pump 5, so that the mass flow ratio of the aldehyde raw material to the ester raw material is 4:6.
the pre-reactor 8, aldehyde raw material and ester raw material according to the weight ratio of 4:6, the mixture enters a pre-reactor 8 in proportion to be preheated and pre-reacted until the bottom of the reactor is mixed with hydrogen, the feeding amount of the hydrogen and the feeding amount are 100 NL/kg, stirring and heating are carried out under the hydrogen condition of the pre-reactor, the reaction of aldehyde and ester is carried out under the condition that solvent ethanol is taken as a carrier, an intermediate product is generated, the hydrogen enters from the bottom of the reactor, the sedimentation problem of a catalyst can be effectively prevented, the reaction rate is accelerated, and the reaction time of the raw materials and the reactor is 1h.
The hydrogen system is characterized in that hydrogen is divided into three parts, one part of the hydrogen is conveyed to the bottom of the pre-reactor through the hydrogen flowmeter, the other part of the hydrogen is conveyed to the bottom of the reactor through the hydrogen flowmeter, and the third part of the hydrogen forms a pressure difference with the hydrogen at the top of the reactor and the hydrogen at the bottom of the reactor, so that the hydrogen system can be used as a detection means for whether serious settlement exists in the reactor. The gravity pressure value of the materials in the reactor can be calculated according to the density of the materials and the height of the reactor to serve as a reference, if the pressure difference is larger than the gravity pressure value, the reactor is blocked, and if the pressure difference is too high, the hydrogen raw material cannot be fed, and the reactor is blocked.
The bottom of the reactor 9 is provided with a stirrer, so that a great amount of catalyst sedimentation and deposition are prevented, the mixing of the solvent and the raw materials is further enhanced, the catalyst is kept homogeneous, the hydrogen gas inlet at the bottom of the reactor 9 enters in a micropore injection mode, the micro-reaction is enhanced, the catalyst is driven to push to the top of the reactor 9, the total feeding of the hydrogen gas and the raw materials in the reactor is 280 NL/kg, and the reaction time in the reactor is 5h.
The gas-liquid separator 10 is provided with a sedimentation pipe, the reacted product conveys the gas-liquid-solid mixture to the lower part of the gas-liquid separator 10, the gas is discharged to a gas recovery system from the top through a gas discharge valve 11 after being separated, and the liquid-solid material at the bottom of the separator is conveyed to a rectifying tower through a liquid level control valve 12 for diversion; the separator is provided with a heat preservation and heating system, a small amount of hydrogen entering from the bottom of the reaction condition can prevent the deposition of a catalyst, and also can promote unreacted substances in the product to further react completely, the top of the separator is provided with a radar liquid level meter, an automatic control system is formed by the radar liquid level meter and a liquid level control valve of the separator, the liquid level is controlled to be an automatic system, and the liquid reaches the automatic valve opening for discharging after the liquid level is set.
The liquid-solid products separated by the rectifying tower 13 and the gas-liquid separator 10 are heated to a certain temperature by a heater at the bottom of the rectifying tower through a liquid level control valve 12 of the separator to separate alkyl ester, aldehyde and ethanol in different tower layers respectively. A part of the product at the bottom of the rectifying tower flows out from the bottom to a catalyst separation system 14 together with the catalyst, and the separated liquid is circulated at the bottom of the rectifying tower 13 by a bottom rectifying tower circulating pump 15.
A method for using a device for producing high-end fine chemical alpha-alkyl ester, which comprises the following steps;
(1) And (3) blowing process gas: the method comprises the steps of filling nitrogen into the top of an ester raw material tank 1 and an aldehyde raw material tank 2, purging the raw material tank and a pump pipeline, adding a temporary pipeline, respectively purging a pre-reactor 8, a reactor 9 and a gas-liquid separator 10 by 1Mpa nitrogen, and purging a rectification system by 0.3Mpa nitrogen;
(3) And (3) cleaning a system: adding 50% of ethanol liquid level into an ester raw material tank 1 and an aldehyde raw material tank 2, starting a stirrer, starting an ester raw material circulating pump 3, an ester raw material feeding pump 4 and an aldehyde raw material feeding pump 5, enabling the ethanol to be filled in a pre-reactor 8 and a reactor 9 according to a feeding ratio of 1:1, starting liquid discharge when the liquid level of a separator is 50%, adding ethanol into a rectifying tower to establish 50% of liquid level, heating to 110 ℃, and washing the tower. The whole system is cleaned by ethanol circulation, and the content of detected impurities is less than or equal to 0.5 percent, which is the cleaning of the system.
(3) Initializing a device: the catalyst in the ester raw material tank 1 and the auxiliary agent are mixed according to a proportion and added into the raw material to 60%, and the ester raw material circulating pump 3 starts circulation; adding raw materials to 60% by weight of the aldehyde raw material tank 2, and starting a raw material tank stirrer; starting a hydrogen system after the airtight of the system is finished, starting the hydrogen system until the purity of the hydrogen reaches 99.9%, adjusting the CO content to be less than or equal to 10ppm, regulating the hydrogen amount of each path, enabling the pressure condition of the system under 2Mpa and the emptying system to be in a stable state, heating the reactor 9 to 65-90 ℃ with the reactor 8, pre-heating the reactor 8, and starting a stirrer of the reactor 9; the separator liquid level was set to 30%; the liquid level of the rectifying tower is established at 45% -50%, the temperature is 60 ℃ -80 ℃, and bottom circulation is established.
(4) The device starts: starting an ester raw material feeding pump 4, an aldehyde raw material feeding pump 5, feeding the mixture of the aldehyde raw material and the ester raw material in a system with a ratio of 4:6, keeping the liquid level of a separator to 35%, keeping the liquid level of a rear rectifying tower to be 45% -50%, gradually heating to 230 ℃ -260 ℃, and separating ethanol 16 and alpha-alkyl ester from the rectifying tower.
(5) The device parks: the system is cooled to normal temperature, the system is depressurized to normal pressure, the ester raw material feed pump 4, the aldehyde raw material feed pump 5 and the ester raw material circulating pump 3 are started to circulate, residual raw materials of the ester raw material tank 1 and the aldehyde raw material tank 2 are discharged from a liquid outlet, products of the pre-reactor 8 and the reactor 9 are discharged, materials of the gas-liquid separator 10 and the rectifying tower 13 are discharged, the system is purged and replaced, and the stopping is finished.
Claims (5)
1. The device for producing the high-end fine chemical alpha-alkyl ester is characterized by comprising an ester raw material tank (1) and an aldehyde raw material tank (2), wherein the top of the ester raw material tank (1) is provided with a variable frequency stirrer, the bottom of the ester raw material tank is connected with an ester raw material circulating pump (3) to form a large amount of circulating raw materials, the variable frequency stirrer is arranged at the bottom of the aldehyde raw material tank (2), the inlet of the ester raw material feeding pump (4) is connected with an outlet pipeline of the ester raw material circulating pump (3), the outlet of the ester raw material feeding pump (4) is provided with an ester raw material feeding flowmeter (6), the feeding amount of the ester is regulated by regulating the stroke and the variable frequency of the ester raw material feeding pump (4), the outlet of the aldehyde raw material tank (2) is connected with the inlet of the aldehyde raw material feeding pump (5), the outlet of the aldehyde raw material feeding pump (5) is an aldehyde raw material feeding flowmeter (7), the feeding amount of aldehyde is regulated by regulating the stroke and frequency conversion of the aldehyde raw material feeding pump (5), the inlet end of the pre-reactor (8) is connected with an ester raw material feeding pump (4) and an outlet pipeline of the aldehyde raw material feeding pump (5), the outlet of the pre-reactor (8) is connected with the inlet end of the reactor (9), the inlet end of the gas-liquid separator (10) is connected with the outlet of the reactor (9), the top of the gas-liquid separator (10) is connected with a gas discharge valve (11), the bottom of the gas-liquid separator (10) is connected with a liquid level control valve (12), and liquid is fed to a rectifying tower (13) through the liquid level control valve (12), the bottom of the rectifying tower (13) is connected with the inlet end of a catalyst separator (14), the outlet of the catalyst separator (14) is connected with the inlet of a rectifying tower circulating pump (15), and the outlet of the rectifying tower circulating pump (15) is connected with a rectifying tower heating kettle to form circulation;
the bottom of the reactor (9) is provided with a stirrer for preventing a large amount of catalyst from sedimentation and deposition, further strengthening the mixing of the solvent and the raw materials, keeping the catalyst homogeneous, enabling hydrogen gas inlet at the bottom of the reactor (9) to enter in a micropore injection mode, strengthening micro-reaction and driving the catalyst to push to the top of the reactor (9).
2. The device for producing high-end fine chemical alpha-alkyl ester according to claim 1, wherein the reactor (9) is a tubular reactor, and a temperature measuring device is arranged inside the reactor; the top and the bottom of the reactor are all flange connection and sealing, a stirrer, a feed inlet and an air inlet are arranged on the flange at the bottom, the flange at the top of the reactor is provided with the air inlet and a material outlet, and a heating device and a heat preservation device are arranged outside the reactor.
3. The device for producing the high-end fine chemical alpha-alkyl ester according to claim 1, wherein the gas-liquid separator (10) is provided with a sedimentation pipe, the reacted product is conveyed to the lower part of the gas-liquid separator (10), the gas is discharged to a gas recovery system from the top through a gas discharge valve (11) after being separated, and the liquid-solid material at the bottom of the gas-liquid separator (10) is sent to a rectifying tower (13) through a liquid level control valve (12) for fractionation; the gas-liquid separator (10) is provided with a heat preservation and heating system, reaction conditions are maintained, a small amount of hydrogen entering from the bottom is used for preventing catalyst deposition and promoting unreacted substances in the product to further react completely, the top of the gas-liquid separator (10) is provided with a radar level gauge, and an automatic control system is formed with a liquid level control valve (12).
4. The device for producing alpha-alkyl ester of high-end fine chemicals according to claim 1, wherein the liquid-solid product separated by the gas-liquid separator (10) is sent to the bottom of the rectifying tower (13) through a separator liquid level control valve (12), the alpha-alkyl ester and the ethanol are separated respectively in different tower layers by heating to a certain temperature through a heater at the bottom of the rectifying tower (13), a part of the product at the bottom of the rectifying tower (13) flows out from the bottom to a catalyst separator (14) together with the catalyst, and the separated liquid is circulated to the bottom of the rectifying tower (13) through a circulating pump (15) of the rectifying tower at the bottom of the tower.
5. A method of using an apparatus for producing alpha-alkyl esters of high-end fine chemicals according to any one of claims 1 to 4, characterized by comprising the steps of;
(1) And (3) blowing process gas: the method comprises the steps of filling nitrogen into the top of an ester raw material tank (1) and an aldehyde raw material tank (2), purging the raw material tank and a pump pipeline, adding a temporary pipeline, respectively purging 1Mpa nitrogen into a pre-reactor (8), a reactor (9) and a gas-liquid separator (10), and purging the rectification system by adopting 0.3Mpa nitrogen;
(2) And (3) cleaning a system: adding 50% of ethanol liquid level into an ester raw material tank (1) and an aldehyde raw material tank (2), starting a stirrer, starting an ester raw material circulating pump (3), an ester raw material feeding pump (4) and an aldehyde raw material feeding pump (5), wherein the feeding ratio is 1:1, enabling ethanol to fill a pre-reactor (8), a reactor (9), a gas-liquid separator (10) with the liquid level of 50% to drain liquid, adding ethanol into a rectifying tower (13) to establish 50% liquid level, heating to 110 ℃, washing the tower, and circularly washing the whole system ethanol, wherein the impurity content is detected to be less than or equal to 0.5% and the system is cleaned;
(3) Initializing a device: the catalyst and the auxiliary agent in the ester raw material tank (1) are mixed in proportion and added into the raw material to 60 percent, and the ester raw material circulating pump (3) starts circulation; adding raw materials to 60% by weight of an aldehyde raw material tank (2), and starting an ester raw material tank (1) stirrer; starting a hydrogen system after the airtight of the system is finished, starting the hydrogen system until the purity of the hydrogen reaches 99.9%, adjusting the CO content to be less than or equal to 10ppm, regulating the hydrogen amount of each path, ensuring that the pressure condition of the system under 2Mpa and the emptying system are in a stable state, preheating a reactor (8), heating a reactor (9) to 65-90 ℃, and starting a stirrer of the pre-reactor (8) and a stirrer of the reactor (9); the liquid level of the gas-liquid separator (10) is set to be 30%; the liquid level of the rectifying tower (13) is established at 45-50%, the temperature is 60-80 ℃, and bottom circulation is established;
(4) The device starts: starting an ester raw material feeding pump (4) and an aldehyde raw material feeding pump (5), wherein the ratio of the aldehyde raw material to the ester raw material is 4:6, feeding the system, the liquid level of a separator is 35%, the liquid level of a rectifying tower (13) is kept at 45% -50%, and gradually heating to 230 ℃ -260 ℃, and separating ethanol and alpha-alkyl ester from the rectifying tower;
(5) The device parks: the system is cooled to normal temperature, the system is depressurized to normal pressure, the ester raw material feed pump (4) and the aldehyde raw material feed pump (5) are stopped, the ester raw material circulating pump (3) is started to circulate, residual raw materials of the ester raw material tank (1) and the aldehyde raw material tank (2) are discharged from a liquid outlet, products of the pre-reactor (8) and the reactor (9) are discharged, materials of the gas-liquid separator (10) and the rectifying tower (13) are discharged, and the system is purged and replaced and stopped.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO1984004103A1 (en) * | 1983-04-18 | 1984-10-25 | Union Carbide Corp | Improved aromatic polyformal blends |
| WO2009054355A1 (en) * | 2007-10-23 | 2009-04-30 | Nippoh Chemicals Co., Ltd. | PROCESS AND APPARATUS FOR PRODUCTION OF CYANOHYDRIN COMPOUND, AND PROCESS FOR PRODUCTION OF α-HYDROXYESTER COMPOUND |
| CN106622040A (en) * | 2017-01-18 | 2017-05-10 | 中国科学院过程工程研究所 | System for preparing acrylic acid and/or acrylic ester by using moving bed reactor and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO1984004103A1 (en) * | 1983-04-18 | 1984-10-25 | Union Carbide Corp | Improved aromatic polyformal blends |
| WO2009054355A1 (en) * | 2007-10-23 | 2009-04-30 | Nippoh Chemicals Co., Ltd. | PROCESS AND APPARATUS FOR PRODUCTION OF CYANOHYDRIN COMPOUND, AND PROCESS FOR PRODUCTION OF α-HYDROXYESTER COMPOUND |
| CN106622040A (en) * | 2017-01-18 | 2017-05-10 | 中国科学院过程工程研究所 | System for preparing acrylic acid and/or acrylic ester by using moving bed reactor and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 纳米Au-CoO_x催化剂的制备及其催化甲基酯化法制备甲基丙烯酸甲酯动力学研究;李国松;王连月;张毅;李文双;姜叶薇;高爽;;石油化工(09);全文 * |
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