CN113185387A - Preparation method of high-purity octabromoether - Google Patents
Preparation method of high-purity octabromoether Download PDFInfo
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- CN113185387A CN113185387A CN202110505083.XA CN202110505083A CN113185387A CN 113185387 A CN113185387 A CN 113185387A CN 202110505083 A CN202110505083 A CN 202110505083A CN 113185387 A CN113185387 A CN 113185387A
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- octabromoether
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- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 54
- 238000005893 bromination reaction Methods 0.000 claims abstract description 41
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims abstract description 28
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052794 bromium Inorganic materials 0.000 claims abstract description 28
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 28
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims abstract description 28
- 238000005406 washing Methods 0.000 claims abstract description 26
- 239000003054 catalyst Substances 0.000 claims abstract description 24
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 24
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000002425 crystallisation Methods 0.000 claims abstract description 21
- 230000008025 crystallization Effects 0.000 claims abstract description 21
- 229960001701 chloroform Drugs 0.000 claims abstract description 20
- 239000000126 substance Substances 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 19
- 230000031709 bromination Effects 0.000 claims abstract description 14
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 14
- 235000010265 sodium sulphite Nutrition 0.000 claims abstract description 14
- -1 tetrabromoether Chemical compound 0.000 claims abstract description 9
- 239000012535 impurity Substances 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 239000013078 crystal Substances 0.000 claims description 12
- ILWRPSCZWQJDMK-UHFFFAOYSA-N triethylazanium;chloride Chemical compound Cl.CCN(CC)CC ILWRPSCZWQJDMK-UHFFFAOYSA-N 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 5
- 230000000694 effects Effects 0.000 abstract description 7
- 238000003912 environmental pollution Methods 0.000 abstract description 6
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 5
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000003063 flame retardant Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- DEIGXXQKDWULML-UHFFFAOYSA-N 1,2,5,6,9,10-hexabromocyclododecane Chemical compound BrC1CCC(Br)C(Br)CCC(Br)C(Br)CCC1Br DEIGXXQKDWULML-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- CMQUQOHNANGDOR-UHFFFAOYSA-N 2,3-dibromo-4-(2,4-dibromo-5-hydroxyphenyl)phenol Chemical compound BrC1=C(Br)C(O)=CC=C1C1=CC(O)=C(Br)C=C1Br CMQUQOHNANGDOR-UHFFFAOYSA-N 0.000 description 1
- 229930188012 Bromoether Natural products 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- HJCMMOODWZOXML-UHFFFAOYSA-N bromo hypobromite Chemical compound BrOBr HJCMMOODWZOXML-UHFFFAOYSA-N 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/18—Preparation of ethers by reactions not forming ether-oxygen bonds
- C07C41/22—Preparation of ethers by reactions not forming ether-oxygen bonds by introduction of halogens; by substitution of halogen atoms by other halogen atoms
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/38—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/40—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/44—Separation; Purification; Stabilisation; Use of additives by treatments giving rise to a chemical modification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystallography & Structural Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the technical field of chemical material synthesis, in particular to a preparation method of high-purity octabromoether, which comprises the steps of firstly preparing bromine, tetrabromoether, trichloromethane or dichloromethane, sodium sulfite and sodium carbonate which are used as raw materials for bromination reaction, then dissolving the tetrabromoether in the dichloromethane or the trichloromethane, then adding bromine, then adding a catalyst into a solution for bromination treatment, then adding the sodium sulfite and the sodium carbonate, then adding a water washing solution, then uniformly stirring, then carrying out centrifugal treatment to stratify the liquid, further removing the water washing solution containing impurities, then carrying out crystallization treatment by adopting a water crystallization mode, and finally carrying out drying treatment to obtain the high-purity octabromoether. The procedures of neutralization and water washing, crystallization, drying and the like are carried out, and the technical effects of reducing environmental pollution, improving purity and reducing cost are realized.
Description
Technical Field
The invention relates to the technical field of chemical material synthesis, in particular to a preparation method of high-purity octabromoether.
Background
Octabromoether is white powder, has low toxicity, can be dissolved in benzene, acetone, chloroform and the like, is insoluble in water and ethanol, has the decomposition temperature of more than 285 ℃, is a main product of tetrabromobisphenol deep processing, and has better flame retardant effect. The octabromoether is used as an additive flame retardant, is a high-efficiency flame retardant containing aromatic bromine and aliphatic bromine, and has excellent thermal stability and light stability. It is mainly used in polypropylene, polypropylene ethylene resin, polyvinyl chloride resin and resin. Compared with hexabromocyclododecane, has higher decomposition temperature, and is not replaced by hexabromocyclododecane in some aspects. The content of octabromoether in industrial synthesis is 90-94%, an auxiliary agent is required to be added in water crystallization, the appearance color is yellowish, and the product stability is poor, so that the preparation method of the high-purity octabromoether is provided for solving the problems.
Disclosure of Invention
The invention aims to provide a preparation method of high-purity octabromoether, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of high-purity octabromoether comprises the following preparation steps:
the method comprises the following steps: preparing raw materials: firstly, preparing raw materials of bromine, tetrabromoether, trichloromethane or dichloromethane for bromination reaction, then preparing sodium sulfite and sodium carbonate for subsequent neutralization reaction, and then independently placing the raw materials for later use;
step two: bromination reaction: then dissolving tetrabromoether in dichloromethane or trichloromethane, then adding bromine, then uniformly stirring, then adding a catalyst into the solution for bromination, and then collecting the solution after bromination for later use;
step three: and (3) neutralization reaction: then adding sodium sulfite and sodium carbonate into the solution obtained in the step two, then uniformly stirring to perform better neutralization reaction, and then collecting the solution obtained for later use;
step four: and (3) water washing treatment: adding a washing solution into the solution obtained in the third step, uniformly stirring, centrifuging to stratify the liquid, removing the washing solution containing impurities, and collecting the rest substances for later use;
step five: and (3) crystallization treatment: then crystallizing the substances collected in the fourth step in a water crystallization mode, and collecting the collected crystals for later use;
step six: drying treatment: and finally, drying the crystals received in the fifth step to obtain the high-purity octabromoether.
Preferably, the content of the effective substances in the step-four bromo ether is more than or equal to 99%.
Preferably, the weight ratio of the tetrabromide, the bromine and the catalyst in the second step is 1028: 500: 1.
preferably, in the second step, when bromine is added dropwise, the temperature of the solution is 10-25 ℃, and when bromination is carried out, the temperature of the solution is 25-35 ℃, and then the temperature is kept for 1-2 hours.
Preferably, the catalyst in the second step is triethylamine hydrochloride.
Preferably, the tetrabromoether is dissolved in dichloromethane in step two.
Preferably, the tetrabromoether is dissolved in chloroform in the second step.
Compared with the prior art, the invention has the beneficial effects that:
the invention discloses a preparation method of octabromoether with low cost and high purity, which realizes the technical effects of reducing environmental pollution, improving purity and reducing cost by the bromination reaction of tetrabromoether, the reaction by adding a catalyst, the procedures of neutralization and water washing, crystallization, drying and the like.
Detailed Description
Example 1: the invention provides a technical scheme that:
a preparation method of high-purity octabromoether comprises the following preparation steps:
the method comprises the following steps: preparing raw materials: firstly, preparing raw materials of bromine, tetrabromoether, trichloromethane or dichloromethane for bromination reaction, then preparing sodium sulfite and sodium carbonate for subsequent neutralization reaction, and then independently placing the raw materials for later use;
step two: bromination reaction: then dissolving tetrabromoether in dichloromethane or trichloromethane, then adding bromine, then uniformly stirring, then adding a catalyst into the solution for bromination, and then collecting the solution after bromination for later use;
step three: and (3) neutralization reaction: then adding sodium sulfite and sodium carbonate into the solution obtained in the step two, then uniformly stirring to perform better neutralization reaction, and then collecting the solution obtained for later use;
step four: and (3) water washing treatment: adding a washing solution into the solution obtained in the third step, uniformly stirring, centrifuging to stratify the liquid, removing the washing solution containing impurities, and collecting the rest substances for later use;
step five: and (3) crystallization treatment: then crystallizing the substances collected in the fourth step in a water crystallization mode, and collecting the collected crystals for later use;
step six: drying treatment: and finally, drying the crystals received in the fifth step to obtain the high-purity octabromoether.
The invention discloses a preparation method of octabromoether with low cost and high purity, which realizes the technical effects of reducing environmental pollution, improving purity and reducing cost by the bromination reaction of tetrabromoether, the reaction by adding a catalyst, the procedures of neutralization and water washing, crystallization, drying and the like.
The content of effective substances in the tetrabromide in the first step is more than or equal to 99 percent, the quality of the octabromoether obtained in the later stage can be effectively ensured by the arrangement, and the weight ratio of the tetrabromide, bromine and the catalyst in the second step is 1028: 500: 1, when dropwise adding bromine in the step two, the temperature of the solution is 10 ℃, when the bromination reaction is carried out, the temperature of the solution is 25 ℃, then the heat preservation time is 2 hours, the better bromination reaction can be guaranteed by the arrangement, the type of the catalyst in the step two is triethylamine hydrochloride, tetrabromoether is dissolved in dichloromethane in the step two.
Example 2: the invention provides a technical scheme that:
a preparation method of high-purity octabromoether comprises the following preparation steps:
the method comprises the following steps: preparing raw materials: firstly, preparing raw materials of bromine, tetrabromoether, trichloromethane or dichloromethane for bromination reaction, then preparing sodium sulfite and sodium carbonate for subsequent neutralization reaction, and then independently placing the raw materials for later use;
step two: bromination reaction: then dissolving tetrabromoether in dichloromethane or trichloromethane, then adding bromine, then uniformly stirring, then adding a catalyst into the solution for bromination, and then collecting the solution after bromination for later use;
step three: and (3) neutralization reaction: then adding sodium sulfite and sodium carbonate into the solution obtained in the step two, then uniformly stirring to perform better neutralization reaction, and then collecting the solution obtained for later use;
step four: and (3) water washing treatment: adding a washing solution into the solution obtained in the third step, uniformly stirring, centrifuging to stratify the liquid, removing the washing solution containing impurities, and collecting the rest substances for later use;
step five: and (3) crystallization treatment: then crystallizing the substances collected in the fourth step in a water crystallization mode, and collecting the collected crystals for later use;
step six: drying treatment: and finally, drying the crystals received in the fifth step to obtain the high-purity octabromoether.
The invention discloses a preparation method of octabromoether with low cost and high purity, which realizes the technical effects of reducing environmental pollution, improving purity and reducing cost by the bromination reaction of tetrabromoether, the reaction by adding a catalyst, the procedures of neutralization and water washing, crystallization, drying and the like.
The content of effective substances in the tetrabromide in the first step is more than or equal to 99 percent, the quality of the octabromoether obtained in the later stage can be effectively ensured by the arrangement, and the weight ratio of the tetrabromide, bromine and the catalyst in the second step is 1028: 500: 1, when adding dropwise bromine in step two, the temperature of solution is 10 degrees centigrade, when carrying out bromination reaction, the 25 degrees centigrade of the temperature of solution, then the time of heat preservation is 2 hours, and better bromination reaction can be guaranteed to this kind of setting, the kind of catalyst is triethylamine hydrochloride in step two, tetrabromoether dissolves in trichloromethane in step two.
Preferably, the tetrabromoether is dissolved in chloroform in the second step.
Example 3: the invention provides a technical scheme that:
a preparation method of high-purity octabromoether comprises the following preparation steps:
the method comprises the following steps: preparing raw materials: firstly, preparing raw materials of bromine, tetrabromoether, trichloromethane or dichloromethane for bromination reaction, then preparing sodium sulfite and sodium carbonate for subsequent neutralization reaction, and then independently placing the raw materials for later use;
step two: bromination reaction: then dissolving tetrabromoether in dichloromethane or trichloromethane, then adding bromine, then uniformly stirring, then adding a catalyst into the solution for bromination, and then collecting the solution after bromination for later use;
step three: and (3) neutralization reaction: then adding sodium sulfite and sodium carbonate into the solution obtained in the step two, then uniformly stirring to perform better neutralization reaction, and then collecting the solution obtained for later use;
step four: and (3) water washing treatment: adding a washing solution into the solution obtained in the third step, uniformly stirring, centrifuging to stratify the liquid, removing the washing solution containing impurities, and collecting the rest substances for later use;
step five: and (3) crystallization treatment: then crystallizing the substances collected in the fourth step in a water crystallization mode, and collecting the collected crystals for later use;
step six: drying treatment: and finally, drying the crystals received in the fifth step to obtain the high-purity octabromoether.
The invention discloses a preparation method of octabromoether with low cost and high purity, which realizes the technical effects of reducing environmental pollution, improving purity and reducing cost by the bromination reaction of tetrabromoether, the reaction by adding a catalyst, the procedures of neutralization and water washing, crystallization, drying and the like.
The content of effective substances in the tetrabromide in the first step is more than or equal to 99 percent, the quality of the octabromoether obtained in the later stage can be effectively ensured by the arrangement, and the weight ratio of the tetrabromide, bromine and the catalyst in the second step is 1028: 500: 1, when dropwise adding bromine in the step two, the temperature of the solution is 25 ℃, and when the bromination reaction is carried out, the temperature of the solution is 35 ℃, and then the heat preservation time is 1 hour, so that the better bromination reaction can be ensured, the type of the catalyst in the step two is triethylamine hydrochloride, and tetrabromoether is dissolved in dichloromethane in the step two.
Example 4: the invention provides a technical scheme that:
a preparation method of high-purity octabromoether comprises the following preparation steps:
the method comprises the following steps: preparing raw materials: firstly, preparing raw materials of bromine, tetrabromoether, trichloromethane or dichloromethane for bromination reaction, then preparing sodium sulfite and sodium carbonate for subsequent neutralization reaction, and then independently placing the raw materials for later use;
step two: bromination reaction: then dissolving tetrabromoether in dichloromethane or trichloromethane, then adding bromine, then uniformly stirring, then adding a catalyst into the solution for bromination, and then collecting the solution after bromination for later use;
step three: and (3) neutralization reaction: then adding sodium sulfite and sodium carbonate into the solution obtained in the step two, then uniformly stirring to perform better neutralization reaction, and then collecting the solution obtained for later use;
step four: and (3) water washing treatment: adding a washing solution into the solution obtained in the third step, uniformly stirring, centrifuging to stratify the liquid, removing the washing solution containing impurities, and collecting the rest substances for later use;
step five: and (3) crystallization treatment: then crystallizing the substances collected in the fourth step in a water crystallization mode, and collecting the collected crystals for later use;
step six: drying treatment: and finally, drying the crystals received in the fifth step to obtain the high-purity octabromoether.
The invention discloses a preparation method of octabromoether with low cost and high purity, which realizes the technical effects of reducing environmental pollution, improving purity and reducing cost by the bromination reaction of tetrabromoether, the reaction by adding a catalyst, the procedures of neutralization and water washing, crystallization, drying and the like.
The content of effective substances in the tetrabromide in the first step is more than or equal to 99 percent, the quality of the octabromoether obtained in the later stage can be effectively ensured by the arrangement, and the weight ratio of the tetrabromide, bromine and the catalyst in the second step is 1028: 500: 1, when adding dropwise bromine in step two, the temperature of solution is 25 degrees centigrade, when carrying out bromination reaction, the 35 degrees centigrade of the temperature of solution, then the time of heat preservation is 1 hour, and better bromination reaction can be guaranteed to this kind of setting, the kind of catalyst is triethylamine hydrochloride in step two, tetrabromoether dissolves in trichloromethane in step two.
The principles and embodiments of the present invention are explained herein using specific examples, which are presented only to assist in understanding the method and its core concepts of the present invention. The foregoing is only a preferred embodiment of the present invention, and it should be noted that there are objectively infinite specific structures due to the limited character expressions, and it will be apparent to those skilled in the art that a plurality of modifications, decorations or changes may be made without departing from the principle of the present invention, and the technical features described above may be combined in a suitable manner; such modifications, variations, combinations, or adaptations of the invention using its spirit and scope, as defined by the claims, may be directed to other uses and embodiments.
Claims (7)
1. A preparation method of high-purity octabromoether is characterized by comprising the following steps: the preparation method comprises the following preparation steps:
the method comprises the following steps: preparing raw materials: firstly, preparing raw materials of bromine, tetrabromoether, trichloromethane or dichloromethane for bromination reaction, then preparing sodium sulfite and sodium carbonate for subsequent neutralization reaction, and then independently placing the raw materials for later use;
step two: bromination reaction: then dissolving tetrabromoether in dichloromethane or trichloromethane, then adding bromine, then uniformly stirring, then adding a catalyst into the solution for bromination, and then collecting the solution after bromination for later use;
step three: and (3) neutralization reaction: then adding sodium sulfite and sodium carbonate into the solution obtained in the step two, then uniformly stirring to perform better neutralization reaction, and then collecting the solution obtained for later use;
step four: and (3) water washing treatment: adding a washing solution into the solution obtained in the third step, uniformly stirring, centrifuging to stratify the liquid, removing the washing solution containing impurities, and collecting the rest substances for later use;
step five: and (3) crystallization treatment: then crystallizing the substances collected in the fourth step in a water crystallization mode, and collecting the collected crystals for later use;
step six: drying treatment: and finally, drying the crystals received in the fifth step to obtain the high-purity octabromoether.
2. The process according to claim 1 for the preparation of high purity octabromoether, wherein: the content of effective substances in the tetrabromoether in the step I is more than or equal to 99 percent.
3. The process according to claim 1 for the preparation of high purity octabromoether, wherein: the weight ratio of the tetrabromoether, bromine and the catalyst in the second step is 1028: 500: 1.
4. the process according to claim 1 for the preparation of high purity octabromoether, wherein: in the second step, when bromine is added dropwise, the temperature of the solution is 10-25 ℃, and when the bromination reaction is carried out, the temperature of the solution is 25-35 ℃, and then the heat preservation time is 1-2 hours.
5. The process according to claim 1 for the preparation of high purity octabromoether, wherein: and the type of the catalyst in the second step is triethylamine hydrochloride.
6. The process according to claim 1 for the preparation of high purity octabromoether, wherein: and in the second step, the tetrabromoether is dissolved in dichloromethane.
7. The process according to claim 1 for the preparation of high purity octabromoether, wherein: and in the second step, the tetrabromoether is dissolved in the trichloromethane.
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| CN115677459A (en) * | 2022-10-27 | 2023-02-03 | 山东博宏新化工科技有限公司 | Crystallization production process of methyl octabromoether |
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| 王彦林等: ""阻燃剂四溴双酚A 双（2,3-二溴丙基）醚的合成研究"", 《海湖盐与化工》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115677459A (en) * | 2022-10-27 | 2023-02-03 | 山东博宏新化工科技有限公司 | Crystallization production process of methyl octabromoether |
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