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Method of synthesizing 1,4-dimethylpiperazine and catalyst used

A technology of dimethylpiperazine and a supported catalyst is applied in the field of synthesizing 1,4-dimethylpiperazine and the catalyst used, and can solve the problem of low atom utilization rate, low economic value, and by-product methylpiperazine. and other problems, to achieve the effect of low cost, suitable reaction conditions and good activity

Inactive Publication Date: 2018-06-22
之江(四川)高新材料应用技术研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, piperazine and formaldehyde are also used to prepare 1,4-dimethylpiperazine, and the yield is 95%. However, both methods will produce methylpiperazine by-product, and the value of piperazine is higher than that of 1,4-dimethylpiperazine. Basepiperazine is higher, so the economic value of this method is not high
[0007] Patent (CN102796061) reports the process of using N,N-dimethylethanolamine as raw material to prepare 1,4-dimethylpiperazine, the yield is 71.1%, but the atomic utilization rate of this method is not high
[0008] The existing process for preparing 1,4-dimethylpiperazine has the disadvantages of three wastes and high production cost

Method used

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  • Method of synthesizing 1,4-dimethylpiperazine and catalyst used
  • Method of synthesizing 1,4-dimethylpiperazine and catalyst used
  • Method of synthesizing 1,4-dimethylpiperazine and catalyst used

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Embodiment 1, a kind of fixed bed reactor, such as figure 1 As shown, it includes a hydrogen cylinder 1, a sample pump 5 and a fixed bed reactor A, and the fixed bed reactor A includes a vaporization chamber 11 and a catalyst bed 6 arranged in sequence from top to bottom, and the middle part of the catalyst bed 6 A catalyst is arranged, and an inert filler 7 is respectively arranged at the upper and lower ends of the catalyst. The outer surface of the catalyst bed 6 is placed in a molten salt bath 8 which is responsible for regulating the reaction temperature in the catalyst bed 6 .

[0036] The outlet of the hydrogen cylinder 1 and the outlet of the sampling pump 5 are connected together to communicate with the top of the vaporization chamber 11; A valve 4 is set between the outlet of 5 and the confluence point; the bottom outlet of the catalyst bed 6 is connected to the condenser 9 and the valve 10 in sequence.

Embodiment 2

[0037] Embodiment 2: the preparation of supported catalyst

[0038] 1) Roasting: Weigh 1000g of spherical γ-Al with a particle diameter of 2-3mm 2 o 3 , calcined at 700°C for 6h to obtain calcined γ-Al 2 o 3 .

[0039] 2) Solution configuration: Weigh 770.5g of copper nitrate trihydrate and 796.3g of nickel nitrate hexahydrate and dissolve them in water, and set the volume to 2500ml to obtain a mixed solution.

[0040] 3), impregnation: the roasted γ-Al obtained in step 1) 2 o 3 Immerse in the solution prepared in step 2), filter after immersing for 24 hours.

[0041] 4), drying: drying the filter cake obtained in step 3) at 100° C. for 8 hours.

[0042] 5) Roasting: the dried product in step 4) is calcined at 500° C. for 8 hours.

[0043] 6), immerse the product of step 5) in the remaining mixed solution after step 3) again, repeat the above steps 3) to 5); repeat 5 times in total, at this time, the mixed solution obtained in step 2) is completely After the absorptio...

Embodiment 3

[0046] Embodiment 3, a kind of method for synthesizing 1,4-dimethylpiperazine, carry out following steps successively:

[0047] 1), get loaded catalyst 300ml and put it in the catalyst bed 6 of the fixed bed reactor as described in embodiment 1,

[0048] First close the valve 4, open the pressure reducing valve 2 and the valve 10, the hydrogen in the hydrogen cylinder 1 flows into the catalyst bed 6, the supported catalyst is activated under the action of hydrogen, the activation temperature is 200°C, the hydrogen pressure is 2MPa, after 24 hours of activation No liquid flows from valve 10, indicating that the supported catalyst has been activated.

[0049] Remarks: The above-mentioned hydrogen pressure is controlled by adjusting the pressure reducing valve 2, the flow meter 3 is used to observe and control the hydrogen flow rate, the sampling pump 5 and valve 4 are closed during activation, the molten salt bath 8 is responsible for controlling the activation temperature, and ...

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Abstract

The invention discloses a supported catalyst for synthesizing 1,4-dimethylpiperazine. Roasted spherical gamma-Al2O3 serves as a carrier, and active components, cuprum and nickel, are loaded on the carrier. The invention further provides a method of synthesizing 1,4-dimethylpiperazine by using the supported catalyst. The method comprises the steps of putting the supported catalyst in a fixed-bed reactor, performing activation by the action of hydrogen, injecting a raw material, N-methylethanolamine into a vaporization chamber via a sampling pump for vaporization, regulating a flow rate of the sampling pump, allowing volumetric space velocity to be 0.1-0.5h<1>, regulating hydrogen pressure to allow reaction pressure to be 0.2-2.0MPa, allowing reaction temperature to be 200-300 DEG C, allowing a product to flow out from the bottom of the fixed-bed reactor, collecting the product after condensation by a condenser, and performing rectification at atmospheric pressure to form 1,4-dimethylpiperazine. The method is simple in technology, appropriate in reaction condition, low in production cost and higher in yield, and the adopted catalyst is low in cost, good in activity and long in service life.

Description

technical field [0001] The invention relates to a method for synthesizing an organic compound 1,4-dimethylpiperazine and a catalyst thereof. Background technique [0002] 1,4-Dimethylpiperazine, which has the formula C 6 h 14 N 2 , the molecular weight is 114, and the structural formula is shown in formula 1, which can be used to synthesize pharmaceutical intermediates, cationic surfactants and polyurethane foam catalysts, etc. [0003] [0004] Literature (Beilstein Journal of Organic Chemistry, 13,329-337; 2017) reported a method for the preparation of 1,4-dimethylpiperazine, using hydroxyethylethylenediamine and methanol as raw materials, using supercritical carbon dioxide as a solvent, γ-Al 2 o 3 As a catalyst, 1,4-dimethylpiperazine was synthesized with a yield of 68%. At the same time, he also reported using the same method to prepare 1,4-dimethylpiperazine with ethanolamine and methanol, with a yield of 13%, most of which were converted into methylmorpholine,...

Claims

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Application Information

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IPC IPC(8): B01J23/755B01J37/02B01J37/08C07D295/023C07D295/03
CPCB01J23/755B01J37/0207B01J37/08C07D295/023C07D295/03
Inventor 张超张哲明张琪张华
Owner 之江(四川)高新材料应用技术研究院有限公司
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