CN112375095B - Continuous process for preparing methylaluminoxane - Google Patents
Continuous process for preparing methylaluminoxane Download PDFInfo
- Publication number
- CN112375095B CN112375095B CN202010805067.8A CN202010805067A CN112375095B CN 112375095 B CN112375095 B CN 112375095B CN 202010805067 A CN202010805067 A CN 202010805067A CN 112375095 B CN112375095 B CN 112375095B
- Authority
- CN
- China
- Prior art keywords
- metering pump
- water
- micro metering
- solvent
- trimethylaluminum
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- CPOFMOWDMVWCLF-UHFFFAOYSA-N methyl(oxo)alumane Chemical compound C[Al]=O CPOFMOWDMVWCLF-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000010924 continuous production Methods 0.000 title claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 64
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000002904 solvent Substances 0.000 claims abstract description 25
- 238000003860 storage Methods 0.000 claims abstract description 18
- 238000002360 preparation method Methods 0.000 claims abstract description 17
- 239000012442 inert solvent Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000000839 emulsion Substances 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 239000003507 refrigerant Substances 0.000 claims description 9
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 239000007788 liquid Substances 0.000 abstract description 3
- 238000012824 chemical production Methods 0.000 abstract description 2
- 239000002920 hazardous waste Substances 0.000 abstract description 2
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical group [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 238000009775 high-speed stirring Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012968 metallocene catalyst Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920005672 polyolefin resin Polymers 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 150000003623 transition metal compounds Chemical class 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/06—Aluminium compounds
- C07F5/061—Aluminium compounds with C-aluminium linkage
- C07F5/066—Aluminium compounds with C-aluminium linkage compounds with Al linked to an element other than Al, C, H or halogen (this includes Al-cyanide linkage)
- C07F5/068—Aluminium compounds with C-aluminium linkage compounds with Al linked to an element other than Al, C, H or halogen (this includes Al-cyanide linkage) preparation of alum(in)oxanes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00002—Chemical plants
- B01J2219/00027—Process aspects
- B01J2219/00033—Continuous processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00873—Heat exchange
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00889—Mixing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00891—Feeding or evacuation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/0095—Control aspects
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
Abstract
The invention discloses a continuous process for preparing methylaluminoxane, which relates to the technical field of chemical production, and aims at the problems of complicated operation steps, poor safety controllability, large hazardous waste amount and high product quality controllability difficulty of the existing intermittent preparation process, the invention provides the following scheme that S1, a microtube reactor, a high-efficiency mixer, a water micro metering pump, a solvent micro metering pump, a trimethylaluminum solution micro metering pump, a pure water storage tank, a solvent storage tank, a trimethylaluminum solution tank and a collection tank are prepared; s2, firstly mixing water and an inert solvent through a high-efficiency mixer to form emulsion, then quickly entering a microtube reactor through a pipeline to react with a trimethylaluminum solution quickly to produce methylaluminoxane, and entering a collecting tank. The invention has safe and controllable technological process, continuous preparation process, narrow temperature control interval in the preparation process, small liquid holdup in the preparation process and good product quality and weight.
Description
Technical Field
The invention relates to the technical field of chemical production, in particular to a continuous process for preparing methylaluminoxane.
Background
The methylaluminoxane is a metallocene catalyst prepared by partially hydrolyzing trimethylaluminum under effective control conditions to form an oligomeric mixture and mixing the oligomeric mixture with a transition metal compound containing a metallocene ring according to a certain proportion, and is used for producing metallocene polyolefin resin. The methylaluminoxane oligomer has different molecular weights and complex structures, the number of aluminum atoms in the molecule is generally varied from 6 to 30, and the structures have linear, annular, trapezoidal, cage-like configurations.
Methylaluminoxane is generally expressed simply as:
various patents have been reported to date on the synthesis of methylaluminoxane, which is largely divided into two categories depending on the source of water used in the preparation process:
the first type uses water of crystallization of inorganic salts or water of adsorption of other substances to hydrolyze trimethylaluminum (CN 102286012A; CN1523027A; CN1165140A; US4665208; US 4544762). Commonly used inorganic salts are, for example, cuSO4.5H20, al2 (SO 4) 3.16H20, fe (SO 4) 2.5H20, etc. The crystallization water compound is used as a water source to prepare methylaluminoxane, so that water molecules are slowly released to react with trimethylaluminum. The addition amount of water can be safely controlled, and the runaway reaction is reduced.
The reaction process has the defect that the release of the total water molecules cannot be accurately calculated, and more seriously, a great amount of dangers (inorganic salt inclusion solvent) are generated in the preparation process. The process has the advantages of poor product repeatability, low yield, complex production process, high cost and difficult industrialization.
The second process is to use purified water as raw material to directly react with trimethylaluminum to prepare methylaluminoxane. CN102190678A and CN1523027a patents report the preparation of methylaluminoxane by emulsifying water with an emulsifier and dispersing in an inert solvent (toluene) in a reaction process with trimethylaluminum. 88108042.X and US4772736 report a process in which a water-added tube is directly introduced into the bottom of a tank of trimethylaluminum solution, and water is dispersed in the solution by high-speed stirring to react with trimethylaluminum to prepare methylaluminoxane. US5041585 reports the preparation of methylaluminoxane by adding water to the liquid level of a trimethylaluminum reactor by high pressure spraying. US5087713 reports that methylaluminoxane is prepared by placing ice cubes in a trimethylaluminum solution kettle at low temperature (-80 ℃), and allowing water molecules on the ice surface to react slowly with trimethylaluminum. US4908463 reports the preparation of methylaluminoxane by mixing water with an inert solvent through a T-tube and then with a trimethylaluminum solution.
The method can accurately calculate the water consumption according to the trimethylaluminum consumption in advance. However, since trimethylaluminum reacts with water severely, the released heat needs to be effectively removed, and water molecules react with trimethylaluminum molecules, so that methylaluminoxane formed in the middle can be further hydrolyzed to form excessive hydrolysis to form aluminum hydroxide, the yield is reduced, and the quality of methylaluminoxane is affected. For this purpose we propose a continuous process for the preparation of methylaluminoxane.
Disclosure of Invention
The invention provides a continuous process for preparing methylaluminoxane, which solves the problems of complex operation steps, poor safety controllability, large hazardous waste amount and high product quality controllability difficulty of the traditional intermittent preparation process.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a process for the continuous preparation of methylaluminoxane comprising the steps of:
s1, preparing a microtube reactor, a high-efficiency mixer, a water micro metering pump, a solvent micro metering pump, a trimethylaluminum solution micro metering pump, a pure water storage tank, a solvent storage tank, a trimethylaluminum solution tank and a collection tank;
s2, firstly mixing water and an inert solvent through a high-efficiency mixer to form emulsion, then quickly entering a microtube reactor through a pipeline to react with a trimethylaluminum solution quickly to produce methylaluminoxane, and entering a collecting tank;
s3, the ratio of water to inert solvent is 1:5 to 1: 15; the feeding speed of water and inert solvent is controlled by a water micro metering pump and a solvent micro metering pump;
s4, controlling the flow rate of pure water to be 5-15 g/min, the precision to be +/-0.1%, the concentration of the trimethylaluminum solution to be 10-20%, controlling the flow rate to be 50-150 ml/m, and controlling the flow rate by a water micro metering pump;
s5, controlling the molar ratio of pure water to trimethylaluminum to be 0.8-1.0:1, controlling the reaction temperature between-15 ℃ and 20 ℃, taking heat released in the reaction process out of a condensation system in a microtube reactor, and selecting the temperature of a refrigerant according to specific temperature requirements.
Preferably, the bottom of the microtube reactor is provided with a refrigerant feeding pipe and a refrigerant discharging pipe.
Preferably, the pure water storage tank is communicated with the water micro metering pump through a pipeline, the solvent storage tank is communicated with the solvent micro metering pump through a pipeline, and the trimethylaluminum solution tank is communicated with the trimethylaluminum solution micro metering pump through a pipeline.
Preferably, the water micro metering pump and the solvent micro metering pump are communicated with the high-efficiency mixer through pipelines.
Preferably, the high-efficiency mixer and the micro metering pump for trimethylaluminum solution are communicated with the microtube reactor through a pipeline.
Preferably, the microtube reactor is configured with a condensing system.
Compared with the prior art, the invention has the beneficial effects that:
the preparation method comprises the steps of (1) safe and controllable technological process, (2) continuous preparation process, (3) narrow temperature control interval in the preparation process, (4) small liquid holdup in the preparation process and (5) good product quality and weight.
Drawings
FIG. 1 is a schematic diagram of a continuous process for preparing methylaluminoxane according to the present invention.
In the figure: 1 a micro-pipe reactor, 2a high-efficiency mixer, 3 a water micro metering pump, 4 a solvent micro metering pump, 5 a trimethylaluminum solution micro metering pump, 6 a pure water storage tank, 7a solvent storage tank, 8a trimethylaluminum solution tank and 9 a collection tank.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments.
Referring to fig. 1, a process for continuously preparing methylaluminoxane comprises the steps of:
s1, preparing a microtube reactor 1, a high-efficiency mixer 2, a water micro metering pump 3, a solvent micro metering pump 4, a trimethylaluminum solution micro metering pump 5, a pure water storage tank 6, a solvent storage tank 7, a trimethylaluminum solution tank 8 and a collection tank 9;
s2, firstly mixing water and an inert solvent through a high-efficiency mixer 2 to form emulsion, then quickly entering a microtube reactor 1 through a pipeline to perform quick reaction with a trimethylaluminum solution to produce methylaluminoxane, and entering a collecting tank 9;
s3, the ratio of water to inert solvent is 1:5 to 1: 15; the feeding speed of water and inert solvent is controlled by a water micro metering pump 3 and a solvent micro metering pump 4;
s4, controlling the flow rate of pure water to be 5-15 g/min, the precision to be +/-0.1%, the concentration of trimethyl aluminum solution to be 10-20%, the flow rate to be 50-150 ml/m, and controlling the flow rate by a water micro metering pump 3;
s5, controlling the molar ratio of pure water to trimethylaluminum to be 0.8-1.0:1, controlling the reaction temperature between-15 ℃ and 20 ℃, taking heat released in the reaction process out of a condensation system in the microtube reactor 1, and selecting the temperature of a refrigerant according to specific temperature requirements.
In this embodiment, the bottom of the micro-pipe reactor 1 is provided with a refrigerant feed pipe and a refrigerant discharge pipe.
In the embodiment, the pure water storage tank 6 is communicated with the water micro metering pump 3 through a pipeline, the solvent storage tank 7 is communicated with the solvent micro metering pump 4 through a pipeline, and the trimethylaluminum solution tank 8 is communicated with the trimethylaluminum solution micro metering pump 5 through a pipeline.
In the embodiment, the water micro metering pump 3 and the solvent micro metering pump 4 are communicated with the high-efficiency mixer 2 through pipelines.
In the embodiment, the high-efficiency mixer 2 and the micro metering pump 5 for trimethylaluminum solution are communicated with the microtube reactor 1 through pipelines.
In this embodiment, the microtube reactor 1 is provided with a condensing system.
Firstly, corresponding raw materials are respectively stored in a pure water storage tank 6, a solvent storage tank 7 and a trimethylaluminum solution tank 8, quantitative and accurate control is carried out on material feeding by using a corresponding metering pump, water and solvent are emulsified by a high-efficiency mixer 2 and then directly react with trimethylaluminum solution in a microtube reactor 1, and the material proportion of methylaluminoxane is produced: the molar ratio of trimethylaluminum to water is between 1:1 and 1:08, the temperature of the reactor is between-15 ℃ and 20 ℃, and the temperature difference is +/-3 ℃, so that the scheme effectively solves the control of the reaction temperature, the molar ratio of trimethylaluminum to water in the reaction process is effectively solved, the reaction process is continuous, the reaction process is stable, the holding amount of the reaction process is small, and the safety and reliability are high.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (2)
1. A process for the continuous preparation of methylaluminoxane comprising the steps of:
s1, preparing a microtube reactor (1), a high-efficiency mixer (2), a water micro metering pump (3), a solvent micro metering pump (4), a trimethylaluminum solution micro metering pump (5), a pure water storage tank (6), a solvent storage tank (7), a trimethylaluminum solution tank (8) and a collection tank (9);
s2, firstly mixing water and an inert solvent through a high-efficiency mixer (2) to form emulsion, then quickly entering a microtube reactor (1) through a pipeline to perform quick reaction with a trimethylaluminum solution to produce methylaluminoxane, and enabling a product to enter a collecting tank (9);
s3, the ratio of water to inert solvent is 1:5 to 1:15; the feeding speed of water and inert solvent is controlled by a water micro metering pump (3) and a solvent micro metering pump (4);
s4, controlling the flow rate of pure water to be 5-15 g/min, the precision to be +/-0.1%, the concentration of the trimethylaluminum solution to be 10-20%, controlling the flow rate to be 50-150 ml/min, and controlling the flow rate by a water micro metering pump (3);
s5, controlling the molar ratio of pure water to trimethylaluminum to be in a range of 0.8-1.0:1, controlling the reaction temperature to be between-15 ℃ and 20 ℃, taking heat released in the reaction process out of a condensation system in the microtube reactor (1), and selecting the temperature of a refrigerant according to specific temperature requirements;
the pure water storage tank (6) is communicated with the water micro metering pump (3) through a pipeline, the solvent storage tank (7) is communicated with the solvent micro metering pump (4) through a pipeline, and the trimethylaluminum solution tank (8) is communicated with the trimethylaluminum solution micro metering pump (5) through a pipeline;
the water micro metering pump (3) and the solvent micro metering pump (4) are communicated with the efficient mixer (2) through pipelines;
the high-efficiency mixer (2) and the micro metering pump (5) for trimethylaluminum solution are communicated with the microtube reactor (1) through pipelines;
the microtube reactor (1) is provided with a condensation system.
2. The continuous process for preparing methylaluminoxane according to claim 1, wherein the bottom of the microtube reactor (1) is provided with a refrigerant feed pipe and a refrigerant discharge pipe.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010805067.8A CN112375095B (en) | 2020-08-12 | 2020-08-12 | Continuous process for preparing methylaluminoxane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010805067.8A CN112375095B (en) | 2020-08-12 | 2020-08-12 | Continuous process for preparing methylaluminoxane |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112375095A CN112375095A (en) | 2021-02-19 |
| CN112375095B true CN112375095B (en) | 2023-04-25 |
Family
ID=74586027
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010805067.8A Active CN112375095B (en) | 2020-08-12 | 2020-08-12 | Continuous process for preparing methylaluminoxane |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112375095B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115121200B (en) * | 2022-07-15 | 2024-02-13 | 浙江大学 | Method for continuously preparing alkylaluminoxane based on micro-membrane reactor |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4908463A (en) * | 1988-12-05 | 1990-03-13 | Ethyl Corporation | Aluminoxane process |
| US4924018A (en) * | 1989-06-26 | 1990-05-08 | Ethyl Corporation | Alkylaluminoxane process |
| CN102190677A (en) * | 2010-03-03 | 2011-09-21 | 中国石油天然气股份有限公司 | Atomization synthesizer and application thereof in synthesis of alkylaluminoxane |
| CN102803280A (en) * | 2009-06-11 | 2012-11-28 | 格雷斯公司 | Process of making aluminoxane and catalysts comprising thus prepared aluminoxane |
| CN109999747A (en) * | 2019-04-23 | 2019-07-12 | 浙江工业大学 | A kind of device and preparation method thereof of serialization preparation adjacent nitro benzyl bromine |
| CN111004265A (en) * | 2018-10-08 | 2020-04-14 | 杭州双安科技有限公司 | Method for preparing alkyl aluminoxane |
-
2020
- 2020-08-12 CN CN202010805067.8A patent/CN112375095B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4908463A (en) * | 1988-12-05 | 1990-03-13 | Ethyl Corporation | Aluminoxane process |
| US4924018A (en) * | 1989-06-26 | 1990-05-08 | Ethyl Corporation | Alkylaluminoxane process |
| CN102803280A (en) * | 2009-06-11 | 2012-11-28 | 格雷斯公司 | Process of making aluminoxane and catalysts comprising thus prepared aluminoxane |
| CN102190677A (en) * | 2010-03-03 | 2011-09-21 | 中国石油天然气股份有限公司 | Atomization synthesizer and application thereof in synthesis of alkylaluminoxane |
| CN111004265A (en) * | 2018-10-08 | 2020-04-14 | 杭州双安科技有限公司 | Method for preparing alkyl aluminoxane |
| CN109999747A (en) * | 2019-04-23 | 2019-07-12 | 浙江工业大学 | A kind of device and preparation method thereof of serialization preparation adjacent nitro benzyl bromine |
Non-Patent Citations (2)
| Title |
|---|
| 朱永新 编著.静态混合器的结构和选用.《柴油机染料特性及其应用技术》.人民交通出版社,1989, * |
| 郭永学 主编.新型微反应器原理与设备.《制药设备与车间设计第3版》.中国健康传媒集团中国医药科技出版社,2019, * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112375095A (en) | 2021-02-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CA2929293C (en) | Production of metal-organic frameworks | |
| CN111647012B (en) | Method for preparing alkylaluminoxane by using microreactor | |
| CN112375095B (en) | Continuous process for preparing methylaluminoxane | |
| CN109134521B (en) | Continuous synthesis method of 2-fluorobenzene boric acid compound | |
| CN111004265A (en) | Method for preparing alkyl aluminoxane | |
| CN105819471A (en) | Method for producing baking soda large in particle size | |
| CN102190678A (en) | Method for preparing modification aluminoxane | |
| CN110713437A (en) | Device and method for preparing oxalic acid by hydrolyzing oxalate | |
| CN112645974B (en) | Controllable preparation method of alkyl aluminoxane | |
| CN214346485U (en) | Tower type reaction device for continuously synthesizing 2-mercaptobenzothiazole | |
| CN106946936B (en) | A method of 2-chloro-2-oxo-1,3,2-dioxaphospholane is synthesized using microchannel continuous flow reactor | |
| CN115121200B (en) | Method for continuously preparing alkylaluminoxane based on micro-membrane reactor | |
| CN110105261A (en) | A method of continuous, rapid synthesis and purification epiphysin using microreactor | |
| CN102351679B (en) | Method for producing crystalline sodium acetate with one-step method | |
| CN114716358A (en) | Method for continuously synthesizing peroxyacetic acid by using microreactor | |
| CN104387258B (en) | A kind of production of chloroacetic acid method and chlorination reactor | |
| CN205074002U (en) | Modified continuous feeding removes hot chemical reactor fast | |
| CN101880293B (en) | Improved production method of N-phosphonomethyl glycine | |
| CN101768059A (en) | Method for continuously formylatelating monoolefine and hydrogen by adopting static mixing reactor | |
| CN113461494B (en) | Method for synthesizing benzenediol by hydroxylation of phenol and hydrogen peroxide | |
| CN115124560A (en) | Method for preparing modified methylaluminoxane by adopting micro-reactor combination through multi-step hydrolysis | |
| CN105170065A (en) | Improved chemical reactor realizing continuous feeding and fast heat removing | |
| CN213085479U (en) | Synthesizer of hydroxylamine hydrochloride | |
| CN220091366U (en) | System for continuously preparing isosorbide dinitrate | |
| CN113292587A (en) | Process for preparing methylaluminoxane |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |