CN110776398A - Benzyl alcohol step pressure hydrolysis reaction process and system - Google Patents
Benzyl alcohol step pressure hydrolysis reaction process and system Download PDFInfo
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- CN110776398A CN110776398A CN201911089976.XA CN201911089976A CN110776398A CN 110776398 A CN110776398 A CN 110776398A CN 201911089976 A CN201911089976 A CN 201911089976A CN 110776398 A CN110776398 A CN 110776398A
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- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 title claims abstract description 132
- 238000006460 hydrolysis reaction Methods 0.000 title claims abstract description 109
- 235000019445 benzyl alcohol Nutrition 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 27
- 230000007062 hydrolysis Effects 0.000 claims abstract description 75
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 46
- KCXMKQUNVWSEMD-UHFFFAOYSA-N benzyl chloride Chemical compound ClCC1=CC=CC=C1 KCXMKQUNVWSEMD-UHFFFAOYSA-N 0.000 claims abstract description 45
- 229940073608 benzyl chloride Drugs 0.000 claims abstract description 45
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims description 42
- 235000017550 sodium carbonate Nutrition 0.000 claims description 14
- 230000003301 hydrolyzing effect Effects 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 abstract description 43
- 239000012043 crude product Substances 0.000 abstract description 28
- 239000000463 material Substances 0.000 abstract description 15
- 239000000047 product Substances 0.000 abstract description 9
- 230000035484 reaction time Effects 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000001816 cooling Methods 0.000 abstract description 6
- MHDVGSVTJDSBDK-UHFFFAOYSA-N dibenzyl ether Chemical compound C=1C=CC=CC=1COCC1=CC=CC=C1 MHDVGSVTJDSBDK-UHFFFAOYSA-N 0.000 abstract description 6
- 238000004821 distillation Methods 0.000 abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 4
- 239000000376 reactant Substances 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
- 239000000243 solution Substances 0.000 description 20
- 239000001569 carbon dioxide Substances 0.000 description 15
- 229910002092 carbon dioxide Inorganic materials 0.000 description 15
- 230000007797 corrosion Effects 0.000 description 9
- 238000005260 corrosion Methods 0.000 description 9
- 239000007791 liquid phase Substances 0.000 description 7
- 230000006837 decompression Effects 0.000 description 6
- 239000003513 alkali Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000010992 reflux 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
- 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
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 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
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 239000012155 injection solvent Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 235000013622 meat product Nutrition 0.000 description 1
- 239000002674 ointment 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
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- 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
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a benzyl alcohol step pressure hydrolysis reaction process and a system, wherein benzyl chloride and sodium carbonate solution are firstly subjected to rapid reaction in a tower reactor under the condition of low pressure, then the content of benzyl chloride in a reactant is further reduced in a hydrolysis kettle under the condition of normal pressure, a benzyl alcohol crude product hydrolysis crude product is obtained, then cooling and continuous oil-water separation are carried out, and an oil phase is subjected to reduced pressure crude distillation and rectification to obtain a product. The method has the production characteristics of mild reaction conditions, short reaction time, low benzyl ether yield and low equipment material requirement, can reduce project construction cost and production cost, and solves the defects of the conventional benzyl alcohol multi-kettle series 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 pressure hydrolysis reaction process technology, benzyl chloride and sodium carbonate solution are subjected to hydrolysis reaction in two combination modes of pressure and normal pressure to prepare benzyl alcohol, and the benzyl alcohol step pressure hydrolysis reaction process has the characteristics of high reaction rate, short reaction time, low byproduct rate, low equipment corrosion rate and the like.
Background
The information in this background section is only for enhancement of 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 that is already known to a person of ordinary skill in the art.
Benzyl alcohol is a colorless liquid, has aromatic flavor, is an important organic chemical raw material, and can be used as a solvent for preparing essence, a coating solvent, a photographic developer, a polyvinyl chloride stabilizer, a medicine synthesis, a synthetic resin solvent, a medicine injection solvent, an antiseptic of ointment or liquid medicine, meat product printing oil, ball-point pen oil and the like.
At present, the main production process of benzyl alcohol is a multi-kettle series normal pressure hydrolysis reaction process, and the process has the characteristics of long reaction time (8-10h), high side yield of benzyl ether, high energy consumption and large specification size of equipment; the continuous production process needs to be carried out under the conditions of high temperature and high pressure, and raw materials such as benzyl chloride, sodium carbonate and the like have high corrosion rate on equipment under the conditions of high temperature and high pressure and have high requirements on equipment materials.
Disclosure of Invention
In order to overcome the problems, the defects of the existing multi-kettle series normal pressure hydrolysis reaction process and the defect of high corrosion rate of the continuous pressurization reaction process to equipment are overcome, so that a high-efficiency and mild reaction condition process scheme is provided, the reaction rate is improved, the yield of the dibenzyl ether is reduced, and the material requirement of the equipment is reduced.
In order to achieve the technical purpose, the technical scheme adopted by the invention is as follows:
a benzyl alcohol step pressure hydrolysis reaction process comprises the following steps:
hydrolyzing part of benzyl chloride under certain pressure to form benzyl alcohol;
hydrolyzing the residual benzyl chloride under normal pressure to form benzyl alcohol.
The research of the invention finds that: the benzyl chloride and the sodium carbonate solution are subjected to hydrolysis reaction by combining pressurization and normal pressure to prepare the benzyl alcohol, and the method has the advantages of high reaction rate, short reaction time, low byproduct rate, low equipment corrosion rate and the like.
In some embodiments, the hydrolysis conditions of the partial benzyl chloride are 120-150 ℃ and 0.2-0.5 MPa under a certain pressure, and most of the benzyl chloride is hydrolyzed under the pressurized condition, so that the yield and the purity of the product are improved.
In some embodiments, the temperature for hydrolyzing the residual benzyl chloride is 95-100 ℃ under normal pressure, so that the unreacted residual benzyl chloride and a small amount of residual benzyl chloride are separated under the pressure in time, and the reaction is continued in the normal pressure reaction kettle.
The invention also provides a system for the pressure hydrolysis reaction of benzyl alcohol, which 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 sequentially connected, 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 after the reaction, the content of benzyl chloride in the hydrolyzed crude product can be reduced to 0.01 percent. The method can be carried out under mild conditions (120-150 ℃ and 0.2-0.5 MPa), reduces the corrosion degree of materials on equipment under a high-temperature and high-pressure state, reduces the reaction time and improves the reaction rate.
In some embodiments, the preheater is arranged on the feeding pipeline of the soda ash, and the subsequent hydrolysis reaction efficiency is improved by increasing the temperature of the alkali liquor during preheating.
The feeding pipeline of the soda ash is connected with the feeding 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 exhaust port 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 extracted carbon dioxide.
In some embodiments, the liquid inlet of the pressurized tower reactor is arranged at the top of the tower and in the middle of the tower, and the heater is arranged between the liquid inlet of the pressurized tower reactor and the liquid outlet at the bottom of the pressurized tower reactor. And (3) decompressing a part of the hydrolysis crude product, then extracting the part of the hydrolysis crude product to a normal-pressure hydrolysis kettle, heating a part of the hydrolysis crude product to 120-150 ℃ by a heater, and then refluxing the part of the hydrolysis crude product to the tower reactor.
In the invention, the pressurized tower reactor only needs to be a tower reactor in the prior benzyl alcohol continuous production method.
In some embodiments, a preheater is arranged between the liquid outlet at the bottom of the pressurized tower reactor and the hydrolysis kettle to heat the materials, so that the reaction efficiency is improved.
In some embodiments, the liquid outlet of the condenser is connected with the liquid inlet of the hydrolysis kettle. Carbon dioxide gas and liquid phase flash steam are sent into a condenser through a riser in the normal pressure hydrolysis kettle, condensate liquid flows back to the normal pressure hydrolysis kettle, and the carbon dioxide gas is recycled.
The specific type and structure of the draft tube are not particularly limited in this application, and those skilled in the art can set the draft tube according to specific working conditions to achieve the purpose of feeding 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 combine production, firstly, the pressurization operation is carried out to remove most of the raw material benzyl chloride, and the residual small amount of benzyl chloride is carried out in a normal pressure reaction kettle. After reaction, the content of benzyl chloride in the hydrolyzed crude product can be reduced to 0.01 percent. The method can be carried out under mild conditions (120-150 ℃ and 0.2-0.5 MPa), reduces the corrosion degree of materials on equipment under a high-temperature and high-pressure state, reduces the reaction time and improves the reaction rate.
(2) The invention provides a benzyl alcohol step pressure hydrolysis reaction process technology, which has the production characteristics of short reaction time, low benzyl ether output rate 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 simple operation method, low cost, universality and easy large-scale production.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a technical schematic diagram of a pressure hydrolysis reaction of benzyl alcohol in example 1.
Wherein, the system comprises 1, benzyl chloride 2, a benzyl chloride feed pump 3, a soda solution 4, a soda feed pump 5, a soda preheater 6, a mixer 7, a pressurized tower reactor 8, a reaction circulating pump 9, a reaction heater 10, a normal pressure hydrolysis kettle 11, a condenser 12, a crude product transfer pump 13 and a benzyl alcohol hydrolysis crude product.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. 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 invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
As introduced in the background art, the reaction time for preparing the benzyl alcohol by the existing batch method is long (8-10h), and the side yield of the benzyl ether is high; the continuous method for preparing the benzyl alcohol has the problems of high temperature, high pressure and serious equipment corrosion. Therefore, the invention provides a benzyl alcohol step pressure hydrolysis reaction process technology, wherein benzyl chloride and soda solution are firstly subjected to rapid reaction in a tower reactor under the condition of low pressure, and then the content of benzyl chloride in a reactant is further reduced in a hydrolysis kettle under the condition of normal pressure, so that a benzyl alcohol crude product is obtained. The method comprises the following specific steps:
1. 10 to 12 percent of soda solution (mass fraction) is pressurized to 0.2 to 0.4MPa by a pump and preheated to 120 to 150 ℃ by a preheater.
2. And (3) the soda ash solution preheated by the preheater and benzyl chloride from a benzyl chloride delivery pump enter a pipeline mixer according to the mass ratio of 1: 4-6, and are fully mixed in the pipeline mixer.
3. And (3) feeding the mixed soda solution and benzyl chloride solution into a benzyl alcohol tower reactor, and carrying out hydrolysis reaction at the temperature of 120-150 ℃ and under the operation condition of 0.2-0.4 MPa.
4. In the step 3, the mixed material of the soda solution and the 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 tower 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 the carbon dioxide.
6. Discharging liquid phase components such as a reactant sodium carbonate solution, benzyl chloride and benzyl alcohol generated by reaction from the bottom of the tower reactor, pressurizing by a pump, extracting a part of hydrolysis crude product to a normal-pressure hydrolysis kettle after reducing pressure, heating a part of hydrolysis crude product to 120-150 ℃ by a heater, and refluxing to the tower reactor, wherein the liquid level of the tower reactor is controlled by the extraction amount.
7. And 6, collecting the crude product of hydrolysis, wherein the content of benzyl chloride in the crude product of hydrolysis is less than or equal to 0.2%, cooling the crude product of hydrolysis by a preheater, feeding the crude product of hydrolysis into a normal-pressure hydrolysis kettle, continuously reacting at the normal pressure and at the temperature of 95-100 ℃, collecting the crude product of hydrolysis when the content of benzyl chloride in the kettle is reduced to 0.05%, cooling and continuously separating oil and water, and carrying out rough reduced-pressure distillation and rectification on an oil phase to obtain the product.
8. Carbon dioxide gas and liquid phase flash steam are sent into a condenser through a riser in the normal pressure hydrolysis kettle, condensate liquid flows back to the normal pressure hydrolysis kettle, and the carbon dioxide gas is recycled.
The present invention is described in further detail below with reference to specific examples, which are intended to be illustrative of the invention and not limiting.
Example 1:
as shown in FIG. 1, 11% soda ash solution (mass fraction) was measured at 0.57m
3The feeding amount per hour is pressurized to 0.3Mpa by a soda conveying pump and then conveyed to a soda preheater, and materials extracted by a tower reactor are preheated to 120 ℃.
As shown in FIG. 1, benzyl chloride is in the range of 0.14m
3The feeding amount is/h, the calcined soda solution which is pressurized by a benzyl chloride delivery pump and preheated enters a pipeline mixer, and the calcined soda solution is fully contacted and mixed in the pipeline mixer and then is delivered to a benzyl alcohol pressurized tower reactor. The reaction materials flow from top to bottom in the tower reactor, and the reaction residence time is 10 minutes. The reaction temperature is 135 ℃ and the reaction pressure is 0.25 MPa.
As shown in fig. 1, the carbon dioxide gas is decompressed by a decompression valve and then is conveyed to a normal pressure hydrolysis kettle for buffering, then is condensed by a condenser and then enters a tail gas treatment system, and condensate liquid flows back to the normal pressure hydrolysis kettle.
As shown in FIG. 1, the liquid phase components such as the soda ash solution, benzyl chloride and benzyl alcohol generated by the reaction were discharged from the bottom of the column reactor, pressurized by a pump, and 0.7m
3The crude hydrolysis product is decompressed and then is extracted to a normal pressure hydrolysis kettle for reaction, the reaction temperature is 98 ℃, and the reaction temperature is 2.0m
3The reaction mixture is heated to 135 ℃ by a heater and then refluxed to the tower reactor.
Extracting a hydrolysis crude product in the normal-pressure hydrolysis kettle by using a pump, cooling, continuously separating oil and water, carrying out reduced pressure rough distillation and rectification on an oil phase to obtain a product, wherein the purity of the product can be more than or equal to 99.95 percent (mass fraction), the yield is more than 90 percent, and the common lining material can meet the use requirement.
Example 2
A benzyl alcohol pressure hydrolysis reaction system comprises: 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 sequentially connected, 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 after the reaction, the content of benzyl chloride in the hydrolyzed crude product can be reduced to 0.01 percent. The method can be carried out under mild conditions (120-150 ℃ and 0.2-0.5 MPa), reduces the corrosion degree of materials on equipment under a high-temperature and high-pressure state, reduces the reaction time and improves the reaction rate.
Example 3
A benzyl alcohol pressure hydrolysis reaction system comprises: 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 sequentially connected, 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 calcined soda, and the subsequent hydrolysis reaction efficiency is improved by increasing the temperature of the alkali liquor during preheating.
Example 4
A benzyl alcohol pressure hydrolysis reaction system comprises: 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 sequentially connected, 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 soda ash 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 pressure hydrolysis reaction system comprises: 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 sequentially connected, 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 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 pressure hydrolysis reaction system comprises: 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 sequentially connected, 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 liquid inlet of the pressurizing tower reactor 7 is 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 pressurizing tower reactor 7 and the liquid outlet at the bottom of the pressurizing tower reactor 7. And (3) decompressing a part of the hydrolysis crude product, then extracting the decompressed hydrolysis crude product to a normal-pressure hydrolysis kettle 10, heating a part of the hydrolysis crude product to 120-150 ℃ by a heater, and then refluxing the heated hydrolysis crude product to a tower reactor 7.
Example 7
A benzyl alcohol pressure hydrolysis reaction system comprises: 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 sequentially connected, 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 pressurizing tower type reactor 7 and the hydrolysis kettle 10 to heat materials, so that the reaction efficiency is improved.
Example 8
A benzyl alcohol pressure hydrolysis reaction system comprises: 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 sequentially connected, 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. Carbon dioxide gas and liquid phase flash steam are sent into a condenser 12 through a riser in the normal pressure hydrolysis kettle 10, condensate liquid flows back to the normal pressure hydrolysis kettle 10, and the carbon dioxide gas is recycled.
Comparative example 1
This comparative example differs from example 1 in that: 0.7m
3The hydrolysis crude product is directly extracted after decompression (no longer carrying out normal pressure reaction), cooling and continuous oil-water separation are carried out, and the product is obtained after the oil phase is subjected to decompression rough distillation and rectification. The benzyl chloride content in the hydrolyzed crude product is between 0.05 and 0.2 percent, which causes raw material loss, and the treatment difficulty of a crude distillation and rectification system is large due to the increase of the benzyl chloride content in the crude product.
Comparative example 2
As shown in FIG. 1, the concentration of 11% soda ash solution is 0.57m
3The feeding amount per hour is pressurized to 0.3Mpa by a soda conveying pump and then conveyed to a soda preheater, and materials extracted by a tower reactor are preheated to 240 ℃.
As shown in FIG. 1, benzyl chloride is in the range of 0.14m
3The feeding amount is/h, the calcined soda solution which is pressurized by a benzyl chloride delivery pump and preheated enters a pipeline mixer, and the calcined soda solution is fully contacted and mixed in the pipeline mixer and then is delivered to a benzyl alcohol pressurized tower reactor. The reaction materials flow from top to bottom in the tower reactor, and the reaction residence time is 10 minutes. The reaction temperature is 270 ℃ and the reaction pressure is 6.5 Mpa.
As shown in fig. 1, the carbon dioxide gas is decompressed by a decompression valve and then is conveyed to a normal pressure hydrolysis kettle for buffering, then is condensed by a condenser and then enters a tail gas treatment system, and condensate liquid flows back to the normal pressure hydrolysis kettle.
Discharging liquid phase components such as sodium carbonate solution, benzyl chloride and benzyl alcohol generated by reaction from the bottom of the tower reactor, pressurizing by pump, and discharging to 2.84m
3The reaction mixture is heated to 270 ℃ by a heater and then flows back to the tower reactor, 0.71m
3And h, extracting the hydrolysis crude product after decompression, cooling, carrying out continuous oil-water separation, and carrying out decompression rough distillation and rectification on the oil phase to obtain the product. The yield of the benzyl alcohol product with the purity of 99.5 percent is about 95 percent, but the requirement on equipment materials is high, and a high-nickel alloy material is required to be used.
It should be noted that the above-mentioned embodiments are only preferred embodiments of the present invention, and the present invention is not limited thereto, and although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications and equivalents can be made in the technical solutions described in the foregoing embodiments, or equivalents thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention. Although the embodiments of the present invention have been described with reference to the accompanying drawings, it is not intended to limit the scope of the present invention, and it should be understood by those skilled in the art that various modifications and variations can be made without inventive efforts by those skilled in the art based on the technical solution of the present invention.
Claims (10)
1. A benzyl alcohol step pressure hydrolysis reaction process is characterized by comprising the following steps:
hydrolyzing part of benzyl chloride under pressure to form benzyl alcohol;
hydrolyzing the residual benzyl chloride under normal pressure to form benzyl alcohol.
2. The benzyl alcohol step pressure hydrolysis reaction process as claimed in claim 1, wherein the partial benzyl chloride is hydrolyzed under pressure at 120-150 ℃ and 0.2-0.5 MPa.
3. The benzyl alcohol step pressure hydrolysis reaction process as claimed in claim 1, wherein the temperature for hydrolyzing the residual benzyl chloride is 95-100 ℃ under normal pressure.
4. A benzyl alcohol step pressure hydrolysis reaction system is characterized by comprising: 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 sequentially connected, and a liquid outlet at the bottom of the pressurized tower reactor is connected with a liquid inlet of the pressurized tower reactor.
5. The system of claim 4, wherein the preheater is disposed on the feed line of soda ash.
6. The system of claim 4, wherein the soda ash feed line is connected in parallel with the benzyl chloride feed line and both are connected to the mixer.
7. The system for the step pressure hydrolysis of benzyl alcohol as recited in claim 4, wherein the gas outlet at the top of the pressurized tower reactor is connected to the hydrolysis kettle.
8. The benzyl alcohol cascade pressure hydrolysis reaction system as claimed in claim 4, wherein the liquid inlet of the pressurized tower reactor is disposed at the top of the tower and at the middle of the tower, and a heater is disposed between the liquid inlet of the pressurized tower reactor and the liquid outlet at the bottom of the pressurized tower reactor.
9. The system for the step pressurized hydrolysis of benzyl alcohol according to claim 4, wherein a preheater is disposed between the liquid outlet at the bottom of the pressurized tower reactor and the hydrolysis kettle.
10. The system of claim 4, wherein the outlet of the condenser is connected to the inlet of the hydrolysis kettle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201911089976.XA CN110776398B (en) | 2019-11-08 | 2019-11-08 | Benzyl alcohol step pressurizing hydrolysis reaction process and system |
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| CN201911089976.XA CN110776398B (en) | 2019-11-08 | 2019-11-08 | Benzyl alcohol step pressurizing hydrolysis reaction process and system |
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| Publication Number | Publication Date |
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| CN110776398A true CN110776398A (en) | 2020-02-11 |
| CN110776398B CN110776398B (en) | 2024-03-22 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115536492A (en) * | 2022-09-29 | 2022-12-30 | 潜江新亿宏有机化工有限公司 | Benzyl alcohol production method and device for reducing consumption of soda ash |
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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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| CN115536492A (en) * | 2022-09-29 | 2022-12-30 | 潜江新亿宏有机化工有限公司 | Benzyl alcohol production method and device for reducing consumption of soda ash |
| CN115536492B (en) * | 2022-09-29 | 2023-12-19 | 潜江新亿宏有机化工有限公司 | Benzyl alcohol production method and device for reducing sodium carbonate consumption |
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