CN113620773A - Method for preparing bromoalkane by catalytic distillation - Google Patents
Method for preparing bromoalkane by catalytic distillation Download PDFInfo
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- CN113620773A CN113620773A CN202110941402.1A CN202110941402A CN113620773A CN 113620773 A CN113620773 A CN 113620773A CN 202110941402 A CN202110941402 A CN 202110941402A CN 113620773 A CN113620773 A CN 113620773A
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- 238000000034 method Methods 0.000 title claims abstract description 29
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 22
- 238000004821 distillation Methods 0.000 title claims abstract description 17
- BMYNFMYTOJXKLE-UHFFFAOYSA-N 3-azaniumyl-2-hydroxypropanoate Chemical compound NCC(O)C(O)=O BMYNFMYTOJXKLE-UHFFFAOYSA-N 0.000 claims abstract description 57
- 238000006243 chemical reaction Methods 0.000 claims abstract description 34
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000003054 catalyst Substances 0.000 claims abstract description 26
- 238000003860 storage Methods 0.000 claims abstract description 24
- 238000010992 reflux Methods 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 9
- 239000000498 cooling water Substances 0.000 claims abstract description 9
- 230000001105 regulatory effect Effects 0.000 claims abstract description 3
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 34
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 18
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 15
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 4
- 239000003377 acid catalyst Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims 1
- 229910052593 corundum Inorganic materials 0.000 claims 1
- 229910001845 yogo sapphire Inorganic materials 0.000 claims 1
- 239000011973 solid acid Substances 0.000 abstract description 10
- 238000000926 separation method Methods 0.000 abstract description 5
- 239000002253 acid Substances 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 3
- 230000007797 corrosion Effects 0.000 abstract description 3
- 150000001298 alcohols Chemical class 0.000 abstract 1
- 150000001347 alkyl bromides Chemical class 0.000 abstract 1
- 238000006555 catalytic reaction Methods 0.000 abstract 1
- 238000000066 reactive distillation Methods 0.000 abstract 1
- CYNYIHKIEHGYOZ-UHFFFAOYSA-N 1-bromopropane Chemical compound CCCBr CYNYIHKIEHGYOZ-UHFFFAOYSA-N 0.000 description 12
- 238000005086 pumping Methods 0.000 description 12
- 238000004817 gas chromatography Methods 0.000 description 7
- 230000001174 ascending effect Effects 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 5
- MPPPKRYCTPRNTB-UHFFFAOYSA-N 1-bromobutane Chemical compound CCCCBr MPPPKRYCTPRNTB-UHFFFAOYSA-N 0.000 description 3
- MPRUWKDQTYKEDP-UHFFFAOYSA-N 3-bromo-2-methylpentane Chemical compound CCC(Br)C(C)C MPRUWKDQTYKEDP-UHFFFAOYSA-N 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 2
- 229910052794 bromium Inorganic materials 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000012847 fine chemical Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000029936 alkylation Effects 0.000 description 1
- 238000005804 alkylation reaction Methods 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 238000006266 etherification reaction Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 239000004434 industrial solvent Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000010977 unit operation Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/093—Preparation of halogenated hydrocarbons by replacement by halogens
- C07C17/16—Preparation of halogenated hydrocarbons by replacement by halogens of hydroxyl groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/383—Separation; Purification; Stabilisation; Use of additives by distillation
-
- 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)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for preparing bromoalkane by catalytic distillation, which comprises the steps of adding low-carbon alcohols into a tower kettle of a reactive distillation tower, and adding hydrobromic acid into the hydrobromic acid from a hydrobromic acid storage tank at the lower part of the distillation tower; a stirring device is arranged at the diameter center of the rectifying tower kettle and below the liquid seal, a storage space is arranged on the surface of the paddle, and the solid acid catalyst is placed in the storage space; introducing cooling water into a condenser at the top of the rectifying tower, opening a heating switch to fill the whole rectifying tower with alcohol steam, and adding hydrobromic acid after the alcohol reaches a stable state in the rectifying tower; regulating reflux ratio, and collecting product bromoalkane from the tower top. According to the invention, the solid acid catalyst is arranged at the stirring paddle, so that the conversion rate of the reaction is improved by using the solid acid catalyst, and meanwhile, the corrosion of the traditional liquid acid to reaction equipment is reduced. The invention integrates catalytic reaction and rectification, directly obtains the target product of alkyl bromide without subsequent treatment such as separation, and finally the conversion rate of alcohols reaches more than 98 percent and the purity of the product reaches more than 99 percent.
Description
Technical Field
The invention belongs to the field of chemical industry, and particularly relates to a method for preparing bromoalkane by catalytic distillation.
Background
Brominated alkanes are important fine chemical raw materials and also are fine chemical products which are greatly demanded in markets at home and abroad, and the brominated alkanes are mainly used for industrial solvents, medicines, pesticides, spices, dyes, surfactants, photosensitive materials and the like. The current methods for producing brominated alkanes mainly comprise two methods: one method is to take bromine as a brominating reagent to react with low-carbon alcohols in the presence of sulfur to prepare bromoalkane, although the process is simpler, bromine is dangerous, and dilute sulfuric acid is generated in the reaction process to generate a large amount of acid water. The other method takes hydrobromic acid and corresponding low-carbon alcohol as raw materials, takes sulfuric acid as a catalyst to synthesize brominated alkanes, can generate a large amount of acid water and wastewater, and is low in yield, low in purity, serious in pollution, complex in post-treatment operation and not in line with green development processes.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a method for preparing bromoalkane by catalytic distillation, which has simple and convenient process, environmental protection and no pollution, and the prepared product has higher purity.
The technical scheme is as follows: the method for preparing brominated alkanes by catalytic distillation comprises the following steps:
(1) adding low-carbon alcohol into a tower kettle of a catalytic rectification tower, and adding hydrobromic acid into the tower from a hydrobromic acid storage tank at the lower part of the rectification tower, so that the quantity ratio of the final substances of the hydrobromic acid to the low-carbon alcohol is 1: 1-8: 1;
(2) installing a stirring device at the diameter center of a rectifying tower kettle and at the position below a liquid seal, and arranging a storage space on the surface of a blade of the stirring device to place a catalyst therein;
(3) introducing cooling water into a condenser at the top of the rectifying tower, opening a heating switch, heating the rectifying tower, keeping full reflux operation after reflux liquid exists at the top of the rectifying tower until the reflux liquid is stable, and then adding hydrobromic acid by a hydrobromic acid feed pump;
(4) regulating reflux ratio, after reaction, collecting product bromoalkane at the tower top, and collecting water, hydrobromic acid and a small amount of alcohol at the tower bottom.
Further, the hydrobromic acid is an aqueous hydrobromic acid solution with the mass fraction of 30-47%.
Further, the low-carbon alcohol is one of propanol, isopropanol and n-butanol with the mass content of 90-100%.
Further, the flow rate of the added hydrobromic acid is 1-3 m3/h。
Further, the position under the liquid seal is 30% -60% of the position under the liquid seal.
Further, the catalyst is a solid strong acid catalyst.
Further, the rectifying tower is heated to control the tower top temperature to be 40-80 ℃ and the tower kettle temperature to be 90-140 ℃.
Further, the reflux ratio is 1-10, and the reaction time is 3-4 h.
Catalytic rectification is a special field in rectification technology, and is a coupled chemical unit operation process which combines chemical reaction and rectification separation in the same equipment, can be used for some traditional processes such as esterification, etherification, hydrogenation, aromatic alkylation and the like, and is one of important methods for strengthening chemical processes. The catalyst has the effect of a tower plate in the reaction process, increases the contact with reactants, and compared with the traditional process, the catalytic rectification obviously reduces the using amount of the catalyst under the condition of reaching the same conversion rate, saves energy and reduces consumption to a certain extent, and has the advantages of high conversion rate, good selectivity, less investment, low energy consumption and the like.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages: the invention provides a process and a device for preparing bromoalkane by catalytic rectification, which integrate reaction and separation into a whole, and compared with the process of separating after the reaction, the method has convenient operation and does not need complicated post-treatment operation; compared with the traditional concentrated sulfuric acid catalyst, the solid strong acid catalyst used in the invention is easy to recover and has little influence on equipment corrosion, the conversion rate of alcohol can reach more than 98%, and the purity of the prepared brominated alkane reaches more than 99%; therefore, compared with the prior art, the preparation process has the advantages of energy conservation, simplicity, convenience, environmental protection, no pollution, convenient operation of the preparation process, low equipment investment, high purity of the prepared brominated alkanes, safety and reliability.
Drawings
FIG. 1 is a schematic diagram of a process unit for preparing brominated alkanes by catalytic distillation.
Detailed Description
The technical scheme of the invention is further explained by combining the attached drawings.
As shown in fig. 1, the device for preparing brominated alkanes by catalytic distillation comprises a rectifying tower 1, a stirring paddle 2, a lower alcohol storage tank 3 and a hydrobromic acid storage tank 5, wherein the lower alcohol storage tank 3 is connected with the tower kettle of the rectifying tower 1 through a lower alcohol feed pump 4, and the hydrobromic acid storage tank 5 is connected with the tower kettle of the rectifying tower 1 through a hydrobromic acid feed pump 6; the middle of the tower kettle of the rectifying tower 1 is provided with a stirring paddle 2, the inside of the tower kettle is filled with a catalyst, the top of the rectifying tower 1 is connected with a condenser 7, and the condenser 7 is connected with a brominated alkane storage tank 8; the bottom of the rectifying tower 1 is connected with a tower bottom liquid recovery tank 9.
Example 1
(1) Pumping 50ml of 99.7% by mass n-propanol from a lower alcohol feed pump 4 to a tower kettle of a rectifying tower 1 through a lower alcohol storage tank 3, and pumping 500ml of 40% by mass hydrobromic acid from a hydrobromic acid storage tank 5 to the tower kettle of the rectifying tower 1 through a hydrobromic acid feed pump 6;
(2) 11g of self-made solid acid catalyst is filled in the stirring paddle 2 of the tower kettle;
(3) after cooling water is introduced into a condenser 7 at the top of the rectifying tower, a heating power supply is turned on, and the temperature is adjusted to 110 ℃ to heat the tower kettle;
(4) adjusting the reflux ratio to be 6, reacting n-propanol and hydrobromic acid under the action of a catalyst to produce bromopropane in a reaction rectification section, ascending to the top of the tower through the rectification section, collecting a product bromopropane at the top of the tower, detecting the content by using a gas chromatography, finally, the mass content of the bromopropane at the top of the tower is more than 99.6%, water, hydrobromic acid and a small amount of n-propanol are added in a tower kettle, and after reacting for 3 hours, the conversion rate of the n-propanol reaches 98%.
Example 2
(1) Pumping 75ml of 99.7% by mass n-propanol from a lower alcohol feed pump 4 to a tower kettle of a rectifying tower 1 through a lower alcohol storage tank 3, and pumping 1000ml of 40% by mass hydrobromic acid from a hydrobromic acid storage tank 5 to the tower kettle of the rectifying tower 1 through a hydrobromic acid feed pump 6;
(2) filling 21.5g of self-made solid acid catalyst at the stirring paddle 2 of the tower kettle;
(3) after cooling water is introduced into a condenser 7 at the top of the rectifying tower, a heating power supply is turned on, and the temperature is adjusted to 110 ℃ to heat the tower kettle;
(4) adjusting the reflux ratio to be 8, reacting n-propanol and hydrobromic acid under the action of a catalyst to produce bromopropane in a reaction rectification section, ascending to the top of the tower through the rectification section, collecting a product bromopropane at the top of the tower, detecting the content by using a gas chromatography, finally, the mass content of the bromopropane at the top of the tower is more than 99.8%, water, hydrobromic acid and a small amount of n-propanol are added in a tower kettle, and after reacting for 3 hours, the conversion rate of the n-propanol reaches 98%.
Example 3
(1) Pumping 50ml of 99.7% by mass n-propanol from a lower alcohol feed pump 4 to a tower kettle of a rectifying tower 1 through a lower alcohol storage tank 3, and pumping 500ml of 40% by mass hydrobromic acid from a hydrobromic acid storage tank 5 to the tower kettle of the rectifying tower 1 through a hydrobromic acid feed pump 6;
(2) 22g of self-made solid acid catalyst is filled in the stirring paddle 2 of the tower kettle;
(3) after cooling water is introduced into a condenser 7 at the top of the rectifying tower, a heating power supply is turned on, and the temperature is adjusted to 110 ℃ to heat the tower kettle;
(4) adjusting the reflux ratio to be 6, reacting n-propanol and hydrobromic acid under the action of a catalyst to produce bromopropane in a reaction rectification section, ascending to the top of the tower through the rectification section, collecting a product bromopropane at the top of the tower, detecting the content by using a gas chromatography, finally, the mass content of the bromopropane at the top of the tower is more than 99.6%, water, hydrobromic acid and a small amount of n-propanol are added in a tower kettle, and after reacting for 3 hours, the conversion rate of the n-propanol reaches 97%.
Example 4
(1) Pumping 50ml of isopropanol with the mass fraction of 99.7% into the tower kettle of the rectifying tower 1 from a lower alcohol feed pump 4 to a lower alcohol storage tank 3, and pumping 500ml of hydrobromic acid with the mass fraction of 40% into a hydrobromic acid storage tank 5 into the tower kettle of the rectifying tower 1 from a hydrobromic acid feed pump 6;
(2) 11g of self-made solid acid catalyst is filled in the stirring paddle 2 of the tower kettle;
(3) after cooling water is introduced into a condenser 7 at the top of the rectifying tower, a heating power supply is turned on, and the temperature is adjusted to 120 ℃ to heat the tower kettle;
(4) adjusting the reflux ratio to 6, reacting isopropanol and hydrobromic acid under the action of a catalyst to produce the isopropyl bromopropane in a reaction rectification section, ascending to the top of the tower through the rectification section, collecting a product of the isopropyl bromopropane at the top of the tower, detecting the content by using a gas chromatography, finally, the content of the isopropyl bromopropane at the top of the tower is more than 99%, the content of water, hydrobromic acid and a small amount of isopropanol in a tower kettle is water, hydrobromic acid and a small amount of isopropanol, and after reacting for 3 hours, the conversion rate of the isopropanol reaches 96%.
Example 5
(1) Pumping 50ml of n-butanol with the mass fraction of 99.7% into the tower kettle of the rectifying tower 1 from a lower alcohol feed pump 4 to a lower alcohol storage tank 3, and pumping 500ml of hydrobromic acid with the mass fraction of 40% into a hydrobromic acid storage tank 5 into the tower kettle of the rectifying tower 1 from a hydrobromic acid feed pump 6;
(2) 11g of self-made solid acid catalyst is filled in the stirring paddle 2 of the tower kettle;
(3) after cooling water is introduced into a condenser 7 at the top of the rectifying tower, a heating power supply is turned on, and the temperature is adjusted to 125 ℃ to heat the tower kettle;
(4) adjusting the reflux ratio to be 6, reacting n-butyl alcohol and hydrobromic acid under the action of a catalyst to produce n-butyl bromide in a reaction rectification section, ascending to the top of the tower through the rectification section, collecting a product n-butyl bromide at the top of the tower, detecting the content by using gas chromatography, wherein the mass content of the n-butyl bromide at the top of the tower is over 98 percent, water, hydrobromic acid and a small amount of n-butyl alcohol are added in a tower kettle, and the conversion rate of the n-butyl alcohol reaches 96 percent after the reaction is carried out for 3 hours.
Comparative example
(1) Pumping 50ml of 99.7% by mass n-propanol from a lower alcohol feed pump 4 to a tower kettle of a rectifying tower 1 through a lower alcohol storage tank 3, and pumping 500ml of 40% by mass hydrobromic acid from a hydrobromic acid storage tank 5 to the tower kettle of the rectifying tower 1 through a hydrobromic acid feed pump 6;
(2) no catalyst is filled in the stirring paddle 2 of the tower kettle;
(3) after cooling water is introduced into a condenser 7 at the top of the rectifying tower, a heating power supply is turned on, and the temperature is adjusted to 110 ℃ to heat the tower kettle;
(4) adjusting the reflux ratio to be 6, reacting n-propanol and hydrobromic acid under the action of a catalyst to produce bromopropane in a reaction rectification section, ascending to the top of the tower through the rectification section, collecting a product bromopropane at the top of the tower, detecting the content by using a gas chromatography, wherein the bromopropane mass content at the top of the tower is over 99.6 percent, water, hydrobromic acid and a small amount of n-propanol are added in a tower kettle, and the conversion rate of the n-propanol is only 67.7 percent after the reaction is carried out for 3 hours.
Therefore, the catalytic distillation with the addition of a proper amount of solid acid catalyst can improve the conversion rate of the reaction, the reaction and the separation are carried out simultaneously, the purity of the product is improved, and the energy consumption is reduced.
The invention heats the tower kettle to ensure that the raw materials are fully contacted, simultaneously, the brominated alkane product with lower boiling point produced by the reaction is enriched to the tower top, and the content is detected by gas chromatography. The invention uses the self-made solid acid catalyst, reduces the corrosion to equipment, is convenient to recover, integrates reaction and rectification into a whole, does not need subsequent treatment operations such as separation and the like, finally enables the conversion rate of low-carbon alcohols to reach more than 98 percent and the product purity to reach more than 99 percent (mass fraction), and realizes the green production of brominated alkanes.
Claims (8)
1. A method for preparing brominated alkanes by catalytic rectification is characterized by comprising the following steps:
(1) adding low-carbon alcohol into a tower kettle of a catalytic rectification tower, and adding hydrobromic acid into the tower from a hydrobromic acid storage tank at the lower part of the rectification tower, so that the quantity ratio of the final substances of the hydrobromic acid to the low-carbon alcohol is 1: 1-8: 1;
(2) installing a stirring device at the diameter center of a rectifying tower kettle and at the position below a liquid seal, and arranging a storage space on the surface of a blade of the stirring device to place a catalyst therein;
(3) introducing cooling water into a condenser at the top of the rectifying tower, opening a heating switch, heating the rectifying tower, keeping full reflux operation after reflux liquid exists at the top of the rectifying tower until the reflux liquid is stable, and then adding hydrobromic acid by a hydrobromic acid feed pump;
(4) regulating reflux ratio, after reaction, collecting product bromoalkane at the tower top, and collecting water, hydrobromic acid and a small amount of alcohol at the tower bottom.
2. The catalytic distillation method for preparing brominated alkanes according to claim 1, wherein in the step (1), the hydrobromic acid is 30-47% of aqueous hydrobromic acid solution by mass fraction.
3. The catalytic distillation method for preparing brominated alkanes according to claim 1, wherein in the step (1), the lower alcohol is one of propanol, isopropanol and n-butanol with the mass content of 90-100%.
4. The catalytic distillation method for preparing brominated alkanes according to claim 1, wherein in the step (1), the flow rate of the added hydrobromic acid is 1-3 m3/h。
5. The catalytic distillation method for preparing brominated alkanes according to claim 1, wherein in the step (2), the position under the liquid seal is 30-60% of the position under the liquid seal.
6. The catalytic distillation method for preparing brominated alkanes according to claim 1, wherein in the step (2), the catalyst is Al2O3/SO4 2-/ZrO2A solid strong acid catalyst.
7. The catalytic distillation method for preparing bromoalkane according to claim 1, wherein in the step (3), the rectifying tower is heated to control the tower top temperature to be 40-80 ℃ and the tower bottom temperature to be 90-140 ℃.
8. The catalytic distillation method for preparing bromoalkane according to claim 1, wherein in the step (4), the reflux ratio is 1-10, and the reaction time is 3-4 h.
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| CN115093305A (en) * | 2022-05-26 | 2022-09-23 | 孟宪锋 | Method for synthesizing dibromoethane by solid acid catalysis |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115093305A (en) * | 2022-05-26 | 2022-09-23 | 孟宪锋 | Method for synthesizing dibromoethane by solid acid catalysis |
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