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Production equipment and preparation technology for o-chlorotoluene Grignard reagent

A technology of o-chlorotoluene and Grignard reagent, which is applied in the field of production equipment and preparation technology of o-chlorotoluene Grignard reagent, can solve problems such as difficult and difficult separation of magnesium chips, and achieve the effect of improving the yield

Active Publication Date: 2015-04-08
SHANGYU HUALUN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The invention provides a production equipment and preparation process of the o-chlorotoluene Grignard reagent, the combination of the production equipment and the preparation process can realize the continuous production of the o-chlorotoluene Grignard reagent, and solve the problems caused by industrial preparation and magnesium chips Difficult separation problem, improved yield of o-chlorotoluene Grignard reagent

Method used

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  • Production equipment and preparation technology for o-chlorotoluene Grignard reagent

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Experimental program
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Effect test

Embodiment 1

[0037] Utilize production equipment among the present invention to prepare o-chlorotoluene Grignard reagent, step is as follows:

[0038] (1) Anhydrous tetrahydrofuran (THF) with a flow rate of 10kg / h, ortho-chlorotoluene and magnesium chips with a flow rate of 5kg / h are passed into the first-level reaction kettle together through the first dip tube, and anhydrous tetrahydrofuran (THF), ortho-chlorotoluene and magnesium Chips are heated up to 65°C while flowing through the first dipping pipe;

[0039] (2) flow is that the anhydrous tetrahydrofuran of 20kg / h, the ortho-chlorotoluene that flow is 10kg / h and the toluene that flow is 10kg / h are passed in the first-level reactor by feed pipe, and step (1) in The mixed liquids are mixed and heated to 80°C to obtain a reaction mixture;

[0040](3) The reaction mixture enters the secondary reaction kettle through the overflow guide pipe of the primary reaction kettle, and is mixed with the incoming magnesium chips, heated to 80°C, an...

Embodiment 2

[0043] Utilize production equipment among the present invention to prepare o-chlorotoluene Grignard reagent, step is as follows:

[0044] (1) Be that the anhydrous tetrahydrofuran of 25kg / h, the ortho-chlorotoluene and the magnesium chips that the flow is 5kg / h are passed into the primary reaction kettle together through the first dipping pipe, anhydrous tetrahydrofuran, ortho-chlorotoluene and magnesium Chips are heated to 70°C while flowing through the first dipping pipe;

[0045] (2) flow is that the anhydrous tetrahydrofuran of 40kg / h, the ortho-chlorotoluene that flow is 10kg / h and the toluene that flow is 15kg / h are passed in the first-level reaction still by feeding pipe, with step (1) The mixed liquids are mixed and heated to 85°C to obtain a reaction mixture;

[0046] (3) The reaction mixture enters the secondary reaction kettle through the overflow guide pipe of the primary reaction kettle, and is mixed with the incoming magnesium chips, heated to 85°C, and the Grig...

Embodiment 3

[0049] Utilize production equipment among the present invention to prepare o-chlorotoluene Grignard reagent, step is as follows:

[0050] (1) Anhydrous tetrahydrofuran (THF) with a flow rate of 20kg / h, ortho-chlorotoluene and magnesium chips with a flow rate of 5kg / h are passed into the first-level reaction kettle together through the first dip tube, and anhydrous tetrahydrofuran (THF), ortho-chlorotoluene and magnesium Chips are heated up to 65°C while flowing through the first dipping pipe;

[0051] (2) flow is that the anhydrous tetrahydrofuran of 30kg / h, the ortho-chlorotoluene that flow is 10kg / h and the toluene that flow is 12kg / h are passed in the first-level reactor by feeding pipe, and step (1) in The mixed liquids are mixed and heated to 85°C to obtain a reaction mixture;

[0052] (3) The reaction mixture enters the secondary reaction kettle through the overflow guide pipe of the primary reaction kettle, and is mixed with the incoming magnesium chips, heated to 85°C...

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Abstract

The invention discloses production equipment and a preparation technology for an o-chlorotoluene Grignard reagent. The equipment comprises a first-stage reaction kettle, a second-stage reaction kettle, a tetrahydrofuran storage tank, an o-chlorotoluene storage tank, a magnesium chip storage tank and a toluene storage tank; the center parts of the first-stage reaction kettle and the second-stage reaction kettle are both provided with a separation net for obstructing magnesium chips; and pipelines are employed for connection of the reaction kettles and the storage tanks. Combination of the continuous production equipment and the corresponding preparation technology for the o-chlorotoluene Grignard reagent solves the problems that initiation is difficult and magnesium chips are difficult to separate in a conventional industrial preparation process of the o-chlorotoluene Grignard reagent, and helps to improve the yield of the o-chlorotoluene Grignard reagent.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a production equipment and preparation process of o-chlorotoluene Grignard reagent. Background technique [0002] Grignard reagent (Grignard reagent) is a class of metal-organic compounds about magnesium discovered by French chemist Grignard in 1901 under the guidance of his teacher Barbie. Since the electronegativity of carbon in the Grignard reagent is greater than that of magnesium, the electron pair on the C-Mg bond is biased towards C, so that the hydrocarbon group is partially charged and the Mg is partially positively charged, which can be compatible with almost all functional groups and many Inorganic compounds can act directly without separation, so Grignard reagents are a kind of nucleophilic reagents, which are widely used in organic synthesis. Grignard reagents are not only widely used analytical reagents and general synthetic reagents in laboratories, but also commo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F3/02B01J19/18
CPCB01J19/18B01J2219/00051C07F3/02
Inventor 李典正何光明孙刚姜嘉宝
Owner SHANGYU HUALUN CHEM
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