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A synthesis method and technology of diquat, applied in the direction of organic chemistry, etc., can solve the problems of complex process, low production efficiency, cumbersome operation, etc.
Active Publication Date: 2021-07-06
NANJING HUAZHOU PHARMA
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[0009] The object of the present invention is to provide a kind of synthetic method and the device of diquat dichloride, to solve the complex process proposed in the above-mentioned background technology, complex operation, production The problem of inefficiency
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[0033] refer to figure 1 , a synthetic method of diquat dichloride, comprising the steps of:
[0034] Step 1: Catalyst Activation
[0035] Put the catalyst into the fixed-bed reactor 4, activate it for 4-6h at a temperature of 300-550°C and a nitrogen flow rate of 50-150ml / min, then lower the temperature to the reaction temperature, and adjust the pressure to the reaction pressure;
[0036] Step 2: Mix the ingredients
[0037] Add dichloroethane and 2,2-bipyridine into mixer 1 and mix, and the temperature of mixer 1 is between 50-100°C;
[0038] Step 3: Cyclization Reaction
[0039] The mixed liquid in the mixer 1 is pumped into the gasification chamber 3 at a certain speed by the centrifugal pump 2 for gasification. After gasification, the gas enters the fixed bed reactor 4 from the top of the fixed bed to react, and the fixed bed reactor 4 then enters the condensation pipe 5 Condensate, water is continuously entered into the condenser pipe 5 to extract diquat dichloride,...
Embodiment 1
[0043] CuO / γ-Al 2 o 3 (the content of CuO is 1%) catalyzer is packed in the fixed-bed reactor, at temperature 300 ℃, activation 4h under the condition of nitrogen flow rate 100ml / min, cool down to 140 ℃, reaction pressure is 1MPa, raw material is 0.5ml / min at speed min into the reactor to react, and then cooled, extracted, separated, distilled and filtered to obtain diquat dichloride product with a yield of 93.5%.
Embodiment 2
[0045] CuO / γ-Al 2 o 3(the content of CuO is 1%) catalyzer is packed in the fixed-bed reactor, at temperature 550 ℃, activation 6h under the condition of nitrogen flow velocity 150ml / min, cool down to 300 ℃, reaction pressure is 3MPa, raw material is 2.5ml / min at speed min into the reactor for reaction, and then cooled, extracted, separated, distilled and filtered to obtain diquat dichloride product with a yield of 91.2%.
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Abstract
The invention discloses a diquat dichloride synthesis method and device. The method comprises the following steps: loading a catalyst into a fixed bed reactor, activating for 4 to 6 hours under the conditions that the temperature is 300 to 550 DEG C and the nitrogen flow rate is 50 to 150 ml / min, and then cooling to the reaction temperature; adding dichloroethane and 2, 2-dipyridyl into a mixer for mixing; pumping a mixed solution in the mixer into a vaporizing chamber at a certain speed through a centrifugal pump to be vaporized, then entering a condensing pipe to be condensed through the fixed bed reactor, enabling water to continuously enter the condensing pipe to extract diquat dichloride, then enabling an extracting solution and raffinate to enter a standing kettle together to be separated, enabling an upper-layer aqueous solution to enter a concentrating kettle to be concentrated, enabling the lower-layer dichloroethane phase to enter a film evaporator to recover dichloroethane and dipyridyl, and preparing the concentrated mixed liquor into diquat mother liquor or diquat mother drug according to requirements. By adopting the continuous production method, the production efficiency is greatly improved, the process is simple, the solvent is convenient to recycle, and the requirement of the reaction on equipment is not high.
Description
technical field [0001] The invention relates to the technical field of herbicide synthesis, in particular to a method and a device for synthesizing diquat dichloride. Background technique [0002] The chemical name of diquat is 1,1'-ethylene-2,2'-bipyridine diium salt, which is an important pyridine herbicide, and its pure product is colorless to light yellow crystal, Developed by the Swiss company Syngenta, it often exists in the form of dibromide monohydrate. At present, the domestic production method of diquat is mainly based on 2,2'-bipyridine and dibromoethane in a tank-type batch reactor The cyclization reaction is carried out in the process, and the single-pass conversion rate of the process is low, the reaction time is long, the utilization rate of the single tank is low, and the reaction efficiency is low. [0003] At present, the industrial method of synthesizing diquat is mainly prepared by reacting 2,2'-bipyridine with dibromoethane, while the preparation of oth...
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