CN110776398B - Benzyl alcohol step pressurizing hydrolysis reaction process and system - Google Patents
Benzyl alcohol step pressurizing hydrolysis reaction process and system Download PDFInfo
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- CN110776398B CN110776398B CN201911089976.XA CN201911089976A CN110776398B CN 110776398 B CN110776398 B CN 110776398B CN 201911089976 A CN201911089976 A CN 201911089976A CN 110776398 B CN110776398 B CN 110776398B
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- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 title claims abstract description 129
- 238000006460 hydrolysis reaction Methods 0.000 title claims abstract description 93
- 235000019445 benzyl alcohol Nutrition 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 21
- 230000007062 hydrolysis Effects 0.000 claims abstract description 61
- KCXMKQUNVWSEMD-UHFFFAOYSA-N benzyl chloride Chemical compound ClCC1=CC=CC=C1 KCXMKQUNVWSEMD-UHFFFAOYSA-N 0.000 claims abstract description 44
- 229940073608 benzyl chloride Drugs 0.000 claims abstract description 44
- 239000007788 liquid Substances 0.000 claims description 36
- 230000003301 hydrolyzing effect Effects 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 abstract description 50
- 238000006243 chemical reaction Methods 0.000 abstract description 42
- 229910000029 sodium carbonate Inorganic materials 0.000 abstract description 23
- 239000012043 crude product Substances 0.000 abstract description 17
- 239000000463 material Substances 0.000 abstract description 12
- 239000000047 product Substances 0.000 abstract description 11
- 230000035484 reaction time Effects 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- MHDVGSVTJDSBDK-UHFFFAOYSA-N dibenzyl ether Chemical compound C=1C=CC=CC=1COCC1=CC=CC=C1 MHDVGSVTJDSBDK-UHFFFAOYSA-N 0.000 abstract description 7
- 230000006837 decompression Effects 0.000 abstract description 6
- 238000004821 distillation Methods 0.000 abstract description 5
- 239000000376 reactant Substances 0.000 abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 4
- 238000001816 cooling Methods 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 3
- 238000010276 construction Methods 0.000 abstract description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 30
- 235000017550 sodium carbonate Nutrition 0.000 description 22
- 239000000243 solution Substances 0.000 description 16
- 239000001569 carbon dioxide Substances 0.000 description 15
- 229910002092 carbon dioxide Inorganic materials 0.000 description 15
- 230000007797 corrosion Effects 0.000 description 10
- 238000005260 corrosion Methods 0.000 description 10
- 239000007791 liquid phase Substances 0.000 description 7
- 239000003513 alkali Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000000605 extraction Methods 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 230000003139 buffering effect Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 description 2
- 239000011541 reaction mixture Substances 0.000 description 2
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 238000011437 continuous method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000012155 injection solvent Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 235000013372 meat Nutrition 0.000 description 1
- 238000010999 medical injection Methods 0.000 description 1
- -1 medical synthesis Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002674 ointment Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/09—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrolysis
- C07C29/12—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrolysis of esters of mineral acids
- C07C29/124—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrolysis of esters of mineral acids of halides
Abstract
The invention relates to a benzyl alcohol step pressurizing hydrolysis reaction process and system, benzyl chloride and sodium carbonate solution are firstly reacted rapidly under the conditions of a tower reactor and low pressure, then the benzyl chloride content in the reactant is further reduced under the conditions of a hydrolysis kettle and normal pressure, the crude product of benzyl alcohol crude hydrolysis is obtained, and then cooling, continuous oil-water separation and oil phase decompression crude distillation and rectification are carried out to obtain the product. The method has the production characteristics of mild reaction conditions, short reaction time, low dibenzyl ether yield and low equipment material requirement, can reduce project construction cost and production cost, and solves the defects of the existing benzyl alcohol multi-kettle serial normal pressure hydrolysis production process and high-temperature high-pressure continuous hydrolysis reaction process.
Description
Technical Field
The invention belongs to a benzyl alcohol step pressurizing hydrolysis reaction process technology, and benzyl chloride and sodium carbonate solution are subjected to hydrolysis reaction in a pressurizing and normal pressure combined mode to prepare benzyl alcohol, and the benzyl alcohol step pressurizing hydrolysis reaction process technology has the characteristics of high reaction rate, short reaction time, low byproduct rate, low equipment corrosion rate and the like.
Background
The disclosure of this background section is only intended to increase the understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art already known to those of ordinary skill in the art.
Benzyl alcohol is colorless liquid, has aromatic smell, is an important organic chemical raw material, and can be used as a solvent for preparing essence, paint solvent, photographic developer, polyvinyl chloride stabilizer, medical synthesis, synthetic resin solvent, medical injection solvent, antiseptic of ointment or medical liquid, meat printing oil, ball-point pen oil and the like.
At present, the main production process of benzyl alcohol is a multi-kettle serial normal pressure hydrolysis reaction process, and the process has the characteristics of long reaction time (8-10 h), high benzyl ether auxiliary yield, high energy consumption and large equipment specification and size; the continuous production process needs to react under high temperature and high pressure conditions, and raw materials such as benzyl chloride, sodium carbonate and the like have high corrosion rate to equipment under high temperature and high pressure conditions, and have high requirements on equipment materials.
Disclosure of Invention
In order to overcome the problems, the prior multi-kettle serial normal pressure hydrolysis reaction process has the defect of high equipment corrosion rate and the defect of high equipment corrosion rate of the continuous pressurizing reaction process, thereby providing a process scheme with high efficiency and mild reaction conditions, improving the reaction rate, reducing the dibenzyl ether yield and reducing the equipment material requirement.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
a benzyl alcohol step-pressurizing hydrolysis reaction process, comprising:
hydrolyzing part of benzyl chloride under a certain pressure to form benzyl alcohol;
and (3) hydrolyzing the residual benzyl chloride to form benzyl alcohol under normal pressure.
The research of the invention finds that: benzyl chloride and sodium carbonate solution are subjected to hydrolysis reaction by the combination of pressurization and normal pressure to prepare benzyl alcohol, and the benzyl alcohol has the advantages of high reaction rate, short reaction time, low byproduct rate, low equipment corrosion rate and the like.
In some embodiments, the conditions for hydrolyzing part of the benzyl chloride are 120-150 ℃ and 0.2-0.5 MPa under certain pressure, and most of the benzyl chloride is hydrolyzed under the condition of pressurization, so that the yield and purity of the product are improved.
In some embodiments, the temperature of the residual benzyl chloride is 95-100 ℃ under normal pressure, the unreacted residual small amount of benzyl chloride is separated from the pressurized condition in time, and the reaction is continued in the normal pressure reaction kettle.
The invention also provides a benzyl alcohol pressurized hydrolysis reaction system, which comprises: the device comprises a preheater, a mixer, a pressurized tower reactor, a heater, a hydrolysis kettle and a condenser; the preheater, the mixer, the pressurized tower reactor, the hydrolysis kettle and the condenser are connected in sequence, and a liquid outlet at the bottom of the pressurized tower reactor is connected with a liquid inlet of the pressurized tower reactor.
The structural design realizes the combination of two reaction modes of pressurization and normal pressure, and the content of benzyl chloride in the hydrolyzed crude product can be reduced to 0.01 percent after the reaction. The invention can be carried out under milder conditions (120-150 ℃ and 0.2-0.5 MPa), reduces the corrosion degree of materials to equipment under high temperature and high pressure, reduces the reaction time and improves the reaction rate.
In some embodiments, the preheater is arranged on the feeding pipeline of the sodium carbonate, and the subsequent hydrolysis reaction efficiency is improved by improving the alkali liquor temperature during preheating.
The feed pipeline of the sodium carbonate is connected with the feed pipeline of the benzyl chloride in parallel and is connected with the mixer, so that the preheated alkali liquor and the benzyl chloride are uniformly mixed in the mixer and then enter the subsequent pressurized tower reactor for hydrolysis reaction, and the reaction efficiency is improved.
In some embodiments, the gas outlet at the top of the pressurized tower reactor is connected with the hydrolysis kettle, so that carbon dioxide gas generated by the hydrolysis reaction is extracted from the top of the tower reactor to the normal pressure hydrolysis kettle, and the pressure of the tower reactor is controlled by the extraction amount of carbon dioxide.
In some embodiments, the liquid inlet of the pressurized tower reactor is respectively arranged at the top of the tower and the middle part of the tower body, and a heater is arranged between the liquid inlet of the pressurized tower reactor and the liquid outlet at the bottom of the pressurized tower reactor. Part of the crude hydrolysis product is decompressed and extracted to an atmospheric hydrolysis kettle, and the other part is heated to 120-150 ℃ by a heater and then flows back to the tower reactor.
In the invention, the pressurized tower reactor is a tower reactor in the current benzyl alcohol continuous method production.
In some embodiments, a preheater is arranged between the liquid outlet at the bottom of the pressurized tower reactor and the hydrolysis kettle, so that materials are heated, and the reaction efficiency is improved.
In some embodiments, the liquid outlet of the condenser is connected to the liquid inlet of the hydrolysis tank. The carbon dioxide gas and liquid phase flash steam are sent into a condenser in the normal pressure hydrolysis kettle through a riser, and condensate liquid flows back to the normal pressure hydrolysis kettle for recycling the carbon dioxide gas.
The specific type and structure of the riser are not particularly limited in this application, and those skilled in the art can set according to specific working conditions to achieve the purpose of delivering carbon dioxide gas and liquid phase flash steam from the hydrolysis kettle to the condenser.
The invention has the beneficial effects that:
(1) The invention adopts two reaction modes of pressurization and normal pressure to produce in a combined way, the majority of raw material benzyl chloride is reacted by pressurization operation, and the rest small amount of benzyl chloride is carried out in a normal pressure reaction kettle. After the reaction, the content of benzyl chloride in the hydrolyzed crude product can be reduced to 0.01 percent. The invention can be carried out under milder conditions (120-150 ℃ and 0.2-0.5 MPa), reduces the corrosion degree of materials to equipment under high temperature and high pressure, reduces the reaction time and improves the reaction rate.
(2) The invention provides a benzyl alcohol step pressurizing hydrolysis reaction process technology, which has the production characteristics of short reaction time, low benzyl ether yield and small equipment corrosion rate, can reduce project construction cost and production cost, and solves the defects of the existing benzyl alcohol production process.
(3) The method has the advantages of simplicity, low cost, universality and easiness in large-scale production.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention.
FIG. 1 is a schematic diagram of the technique of the benzyl alcohol pressure hydrolysis reaction of example 1.
Wherein, 1, benzyl chloride 2, benzyl chloride feed pump 3, soda solution 4, soda feed pump 5, soda preheater 6, mixer 7, pressurized tower reactor 8, reaction circulating pump 9, reaction heater 10, normal pressure hydrolysis kettle 11, condenser 12, crude product transfer pump 13, benzyl alcohol hydrolysis crude product.
Detailed Description
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the invention. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the present invention. As used herein, the singular is also intended to include the plural unless the context clearly indicates otherwise, and furthermore, it is to be understood that the terms "comprises" and/or "comprising" when used in this specification are taken to specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof.
As described in the background art, the reaction time for preparing benzyl alcohol by the current batch method is long (8-10 h), and the side yield of benzyl ether is high; the continuous process for preparing benzyl alcohol has high temperature, high pressure and serious equipment corrosion. Therefore, the invention provides a benzyl alcohol step pressurizing hydrolysis reaction process technology, benzyl chloride and sodium carbonate solution firstly react rapidly under the conditions of a tower reactor and low pressure, and then the benzyl chloride content in the reactant is further reduced under the conditions of a hydrolysis kettle and normal pressure, so as to obtain a benzyl alcohol crude product. The method comprises the following specific steps:
1. 10 to 12 percent of sodium carbonate solution (mass fraction) is pressurized to 0.2 to 0.4MPa by a pump and preheated to 120 to 150 ℃ by a preheater.
2. The sodium carbonate solution preheated by the preheater and benzyl chloride from the benzyl chloride conveying pump enter a pipeline mixer according to the mass ratio of 1:4-6, and are fully mixed in the pipeline mixer.
3. The mixed sodium carbonate solution and benzyl chloride solution enter a benzyl alcohol tower reactor to carry out hydrolysis reaction under the operation condition of 120-150 ℃ and 0.2-0.4 MPa.
4. In the step 3, the mixture of sodium carbonate solution and benzyl chloride enters from the top of the tower reactor and flows through the reaction zone from top to bottom in the tower reactor.
5. Carbon dioxide gas generated by the reaction is extracted from the top of the tower reactor to the normal pressure hydrolysis kettle, and the pressure of the tower reactor is controlled by the extraction amount of carbon dioxide.
6. Liquid phase components such as reactant sodium carbonate solution, benzyl chloride and benzyl alcohol generated by reaction are discharged from the bottom of the tower reactor, pressurized by a pump, part of hydrolysis crude products are decompressed and extracted to an atmospheric hydrolysis kettle, and part of hydrolysis crude products are heated to 120-150 ℃ by a heater and then flow back to the tower reactor, and the liquid level of the tower reactor is controlled by the extraction amount.
7. In the step 6, the benzyl chloride content in the extracted hydrolysis crude product is less than or equal to 0.2%, the hydrolysis crude product enters an atmospheric hydrolysis kettle after being cooled by a preheater, the reaction is continued under the atmospheric pressure and at the temperature of 95-100 ℃, the benzyl chloride content in the kettle is extracted when the benzyl chloride content in the kettle is reduced to 0.05%, the hydrolysis crude product is cooled, continuous oil-water separation is carried out, and the oil phase is subjected to reduced pressure crude distillation and rectification to obtain the product.
8. The carbon dioxide gas and liquid phase flash steam are sent into a condenser in the normal pressure hydrolysis kettle through a riser, and condensate liquid flows back to the normal pressure hydrolysis kettle for recycling the carbon dioxide gas.
The invention will now be described in further detail with reference to the following specific examples, which should be construed as illustrative rather than limiting.
Example 1:
as shown in FIG. 1, 11% soda ash solution(mass fraction) according to 0.57m 3 And (3) pressurizing the feed quantity per hour by a soda ash conveying pump to 0.3Mpa, conveying the feed quantity to a soda ash preheater, and preheating the extracted material to 120 ℃ by using a tower reactor.
As shown in FIG. 1, benzyl chloride was added at 0.14m 3 And (3) the feeding amount of/h, namely, the sodium carbonate solution after being pressurized by a benzyl chloride conveying pump and preheated enters a pipeline mixer, and is conveyed to a benzyl alcohol pressurized tower reactor after being fully contacted and mixed in the pipeline mixer. The reaction mass flowed from top to bottom in the column reactor with a reaction residence time of 10 minutes. The reaction temperature is 135 ℃ and the reaction pressure is 0.25Mpa.
As shown in fig. 1, the carbon dioxide gas is decompressed by a decompression valve and then is conveyed to an atmospheric pressure hydrolysis kettle for buffering, and then is condensed by a condenser and then enters a tail gas treatment system, and condensate flows back to the atmospheric pressure hydrolysis kettle.
As shown in FIG. 1, the liquid phase components such as the reactant soda ash solution, benzyl chloride and benzyl alcohol generated by the reaction are discharged from the bottom of the tower reactor, pressurized by a pump, and the pressure is 0.7m 3 The/h hydrolysis crude product is decompressed and is extracted to a normal pressure hydrolysis kettle for reaction, the reaction temperature is 98 ℃ and the reaction temperature is 2.0m 3 The reaction mixture was heated to 135℃by a heater and refluxed to the column reactor.
The crude hydrolysis product in the normal pressure hydrolysis kettle is extracted by a pump, is cooled and subjected to continuous oil-water separation, and the oil phase is subjected to reduced pressure crude distillation and rectification to obtain the product, wherein the purity of the product can be more than or equal to 99.95% (mass fraction), the yield is more than 90%, and the common lining material can meet the use requirement.
Example 2
A benzyl alcohol pressurized hydrolysis reaction system comprising: a preheater 5, a mixer 6, a pressurized tower reactor 7, a heater 9, a hydrolysis kettle 10 and a condenser 12; the preheater 5, the mixer 6, the pressurized tower reactor 7, the hydrolysis kettle 10 and the condenser 12 are connected in sequence, and a liquid outlet at the bottom of the pressurized tower reactor 7 is connected with a liquid inlet of the pressurized tower reactor 7.
The structural design realizes the combination of two reaction modes of pressurization and normal pressure, and the content of benzyl chloride in the hydrolyzed crude product can be reduced to 0.01 percent after the reaction. The invention can be carried out under milder conditions (120-150 ℃ and 0.2-0.5 MPa), reduces the corrosion degree of materials to equipment under high temperature and high pressure, reduces the reaction time and improves the reaction rate.
Example 3
A benzyl alcohol pressurized hydrolysis reaction system comprising: a preheater 5, a mixer 6, a pressurized tower reactor 7, a heater 9, a hydrolysis kettle 10 and a condenser 12; the preheater 5, the mixer 6, the pressurized tower reactor 7, the hydrolysis kettle 10 and the condenser 12 are connected in sequence, and a liquid outlet at the bottom of the pressurized tower reactor 7 is connected with a liquid inlet of the pressurized tower reactor 7.
The preheater 5 is arranged on the feed pipeline of the sodium carbonate, and the subsequent hydrolysis reaction efficiency is improved by improving the alkali liquor temperature during preheating.
Example 4
A benzyl alcohol pressurized hydrolysis reaction system comprising: a preheater 5, a mixer 6, a pressurized tower reactor 7, a heater 9, a hydrolysis kettle 10 and a condenser 12; the preheater 5, the mixer 6, the pressurized tower reactor 7, the hydrolysis kettle 10 and the condenser 12 are connected in sequence, and a liquid outlet at the bottom of the pressurized tower reactor 7 is connected with a liquid inlet of the pressurized tower reactor 7.
The feed pipeline of the sodium carbonate is connected with the feed pipeline of the benzyl chloride in parallel and is connected with the mixer 6, so that the preheated alkali liquor and the benzyl chloride are uniformly mixed in the mixer 6 and then enter the subsequent pressurized tower reactor 7 for hydrolysis reaction, and the reaction efficiency is improved.
Example 5
A benzyl alcohol pressurized hydrolysis reaction system comprising: a preheater 5, a mixer 6, a pressurized tower reactor 7, a heater 9, a hydrolysis kettle 10 and a condenser 12; the preheater 5, the mixer 6, the pressurized tower reactor 7, the hydrolysis kettle 10 and the condenser 12 are connected in sequence, and a liquid outlet at the bottom of the pressurized tower reactor 7 is connected with a liquid inlet of the pressurized tower reactor 7.
The exhaust port at the top of the pressurized tower reactor 7 is connected with the hydrolysis kettle 10, so that carbon dioxide gas generated by the hydrolysis reaction is extracted from the top of the tower reactor 7 to the normal pressure hydrolysis kettle 10, and the pressure of the tower reactor 7 is controlled by the extraction amount of carbon dioxide.
Example 6
A benzyl alcohol pressurized hydrolysis reaction system comprising: a preheater 5, a mixer 6, a pressurized tower reactor 7, a heater 9, a hydrolysis kettle 10 and a condenser 12; the preheater 5, the mixer 6, the pressurized tower reactor 7, the hydrolysis kettle 10 and the condenser 12 are connected in sequence, and a liquid outlet at the bottom of the pressurized tower reactor 7 is connected with a liquid inlet of the pressurized tower reactor 7.
The liquid inlets of the pressurized tower reactor 7 are respectively arranged at the top of the tower and the middle part of the tower body, and a heater 9 is arranged between the liquid inlet of the pressurized tower reactor 7 and the liquid outlet at the bottom of the pressurized tower reactor 7. Part of the crude hydrolysis product is decompressed and extracted to the normal pressure hydrolysis kettle 10, and part is heated to 120-150 ℃ by a heater and then flows back to the tower reactor 7.
Example 7
A benzyl alcohol pressurized hydrolysis reaction system comprising: a preheater 5, a mixer 6, a pressurized tower reactor 7, a heater 9, a hydrolysis kettle 10 and a condenser 12; the preheater 5, the mixer 6, the pressurized tower reactor 7, the hydrolysis kettle 10 and the condenser 12 are connected in sequence, and a liquid outlet at the bottom of the pressurized tower reactor 7 is connected with a liquid inlet of the pressurized tower reactor 7.
A preheater 5 is arranged between a liquid outlet at the bottom of the pressurized tower reactor 7 and the hydrolysis kettle 10 to heat materials, so that the reaction efficiency is improved.
Example 8
A benzyl alcohol pressurized hydrolysis reaction system comprising: a preheater 5, a mixer 6, a pressurized tower reactor 7, a heater 9, a hydrolysis kettle 10 and a condenser 12; the preheater 5, the mixer 6, the pressurized tower reactor 7, the hydrolysis kettle 10 and the condenser 12 are connected in sequence, and a liquid outlet at the bottom of the pressurized tower reactor 7 is connected with a liquid inlet of the pressurized tower reactor 7.
The liquid outlet of the condenser 12 is connected with the liquid inlet of the hydrolysis kettle. The carbon dioxide gas and liquid phase flash steam are sent into a condenser 12 in the normal pressure hydrolysis kettle 10 through a riser, and condensate flows back to the normal pressure hydrolysis kettle 10 for recycling the carbon dioxide gas.
Comparative example 1
This comparative example differs from example 1 in that: 0.7m 3 And (3) directly extracting the hydrolyzed crude product after decompression (no longer carrying out normal pressure reaction), cooling, continuously separating oil from water, and rectifying the oil phase to obtain the product after decompression crude distillation. The benzyl chloride content in the hydrolyzed crude product is between 0.05 and 0.2 percent, which causes raw material loss, and the increase of the benzyl chloride content in the crude product causes great difficulty in the treatment of a crude distillation and rectification system.
Comparative example 2
As shown in FIG. 1, the 11% soda ash solution was prepared at 0.57m 3 And (3) pressurizing the feed quantity per hour by a soda ash conveying pump to 0.3Mpa, conveying the feed quantity to a soda ash preheater, and preheating the extracted material to 240 ℃ by using a tower reactor.
As shown in FIG. 1, benzyl chloride was added at 0.14m 3 And (3) the feeding amount of/h, namely, the sodium carbonate solution after being pressurized by a benzyl chloride conveying pump and preheated enters a pipeline mixer, and is conveyed to a benzyl alcohol pressurized tower reactor after being fully contacted and mixed in the pipeline mixer. The reaction mass flowed from top to bottom in the column reactor with a reaction residence time of 10 minutes. The reaction temperature is 270 ℃ and the reaction pressure is 6.5Mpa.
As shown in fig. 1, the carbon dioxide gas is decompressed by a decompression valve and then is conveyed to an atmospheric pressure hydrolysis kettle for buffering, and then is condensed by a condenser and then enters a tail gas treatment system, and condensate flows back to the atmospheric pressure hydrolysis kettle.
Liquid phase components such as reactant soda solution, benzyl chloride and benzyl alcohol generated by the reaction are discharged from the bottom of the tower reactor, pressurized by a pump for 2.84m 3 The reaction mixture was heated to 270℃by a heater and refluxed to the column reactor at 0.71m 3 And (3) extracting the hydrolyzed crude product after decompression, cooling, separating continuous oil from water, and rectifying the oil phase to obtain the product. The benzyl alcohol product with the purity of 99.5 percent has the yield of about 95 percent, but has high requirements on equipment materials, and high nickel alloy materials are needed.
Finally, it should be noted that the above-mentioned embodiments are only preferred embodiments of the present invention, and the present invention is not limited to the above-mentioned embodiments, but may be modified or substituted for some of them by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention. While the foregoing description of the embodiments of the present invention has been presented in conjunction with the drawings, it should be understood that it is not intended to limit the scope of the invention, but rather, it is intended to cover all modifications or variations within the scope of the invention as defined by the claims of the present invention.
Claims (1)
1. The benzyl alcohol step pressurizing hydrolysis process is characterized by comprising the following steps:
hydrolyzing part of benzyl chloride under the condition of pressurization to form benzyl alcohol;
hydrolyzing the residual benzyl chloride to form benzyl alcohol under normal pressure;
the specific operation of the benzyl alcohol step pressurizing hydrolysis reaction process is controlled by a benzyl alcohol step pressurizing hydrolysis reaction system, and the benzyl alcohol step pressurizing hydrolysis reaction system comprises a preheater, a mixer, a pressurizing tower reactor, a heater, a hydrolyzing kettle and a condenser;
the liquid inlets of the pressurized tower reactor are respectively arranged at the top of the tower and the middle part of the tower body, and a heater is arranged between the liquid inlet of the pressurized tower reactor and the liquid outlet at the bottom of the pressurized tower reactor; part of the crude hydrolysis product is decompressed and then extracted to an atmospheric hydrolysis kettle, and the other part is heated to 120-150 ℃ by a heater and then flows back to a tower reactor;
under the condition of pressurization, the condition of partial benzyl chloride hydrolysis is 120-150 ℃ and 0.2-0.5 MPa;
the temperature of the residual benzyl chloride is set to 95-100 ℃ under normal pressure.
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| CN101811936A (en) * | 2009-11-12 | 2010-08-25 | 山东聊城中盛蓝瑞化工有限公司 | Benzyl alcohol continuous hydrolysis technology and use equipment thereof |
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