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Preparation method of N-alkylated triamine-based star-like ultra-low molecular inhibitor

A technology for alkylation of triamine-based star and ultra-low molecular weight, which is applied in the fields of reductive alkylation preparation, chemical instruments and methods, organic chemistry, etc., can solve the problems of unfavorable safety, lengthy preparation route, cumbersome intermediate steps and the like, Accurate and controllable molecular size and structure, simple process and low cost

Active Publication Date: 2019-06-21
YANGTZE UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Nitrilotriacetic acid itself is a flammable substance with a strong pungent smell, and its preparation route is tedious, and the intermediate steps are cumbersome. Catalytic hydrogenation under normal pressure conditions, and inflammable and explosive metal hydrides, such as lithium aluminum hydride, etc., are required to carry out the reaction under normal pressure conditions, which is not conducive to the safe conduct of the experiment.

Method used

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  • Preparation method of N-alkylated triamine-based star-like ultra-low molecular inhibitor
  • Preparation method of N-alkylated triamine-based star-like ultra-low molecular inhibitor
  • Preparation method of N-alkylated triamine-based star-like ultra-low molecular inhibitor

Examples

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Embodiment 1

[0026] This example is a preparation example of the PCC reagent. It should be noted that in the field of chemistry, the PCC reagent is a complex salt solution of chromium trioxide and pyridine in hydrochloric acid.

[0027] Quickly add 100 g of chromium trioxide to 184 mL of hydrochloric acid with a concentration of 6 mol / L (which contains 1.1 mol of HCl) while stirring, and after 5 min, cool the homogeneous solution to 0°C to obtain a reddish-brown liquid, which is removed by filtration under normal pressure. Insolubles. Afterwards, within 10 minutes, 79.1 g of pyridine was added to the homogeneous solution. With the addition of pyridine, a yellow solid gradually precipitated. After the pyridine was added dropwise, it was cooled to 0°C again to obtain an orange solid, which was collected by filtration with a sand core funnel. Yellow solid product. The product was dried in a vacuum desiccator for 1 hour, and then dried in a desiccator filled with phosphorus pentoxide for 48 h...

Embodiment 2

[0031] This example is a preparation example of 1,1,1-triacetaldehyde amine.

[0032] dichloromethane (DCM) over anhydrous CaCl 2 After drying, re-evaporate, and then dissolve the PCC reagent in the DCM after re-distillation to remove water and stir. After the PCC reagent is completely dissolved, pour it into a 500mL three-necked flask. Add the DCM solution of triethanolamine dropwise to the three-necked flask under stirring at room temperature to ensure that the molar ratio of the hydroxyl group of triethanolamine to the PCC reagent is 1:1.5, and continue to react for 4 hours after the dropwise addition is completed, then stop the reaction. Pour out the upper layer solution, wash the lower layer of solid matter with DCM 3 times, combine the upper layer solution and the washing solution, and wash the solution with saturated NaHCO successively 3 Washed with aqueous solution, followed by anhydrous Na 2 SO 4 After drying and filtering to remove the solvent, the residual liquid...

Embodiment 3

[0038] This example is a preparation example of 1,1,1-triaminoethylamine.

[0039] Weigh ammonium formate and formic acid according to the molar ratio of 1:2, stir well and pour into excess toluene, stir again and pour into a three-necked flask with a condensing reflux tube. After the temperature was raised to 80° C. under the condition of an oil bath, a toluene solution of 1,1,1-triacetaldehyde amine was added dropwise into the three-necked flask. After the dropwise addition, the temperature of the reaction solution system was slowly raised to 160°C, the reaction was continued for 6 hours, and then the reaction was stopped to obtain a black tar-like liquid. 3 Wash with saturated NaCl aqueous solution, and the liquid after layering is separated with a separatory funnel, and washed with anhydrous NaCl 2 SO 4 The upper mother liquor was dried, and finally the residue was distilled under reduced pressure to obtain white needle-like crystals, namely 1,1,1-triaminoethylamine (TAE...

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Abstract

The invention discloses a preparation method of an N-alkylated triamine-based star-like ultra-low molecular inhibitor. The preparation method comprises the following steps: taking triethanolamine as araw material and sequentially performing oxidation reaction and amination reaction on the triethanolamine in a solution to obtain a final product. The preparation method is simple in process, low incost, mild in conditions, good in safety, high in yield and suitable for industrial production. The N-alkylated triamine-based star-like ultra-low molecular inhibitor prepared by the method disclosedby the invention has the characteristics that the molecular size and the structure are precisely controllable, a terminal group is a primary amine group, and the group density is large, has a strong inhibition effect on hydration pulping of bentonite and mud shale, can effectively inhibit the hydration expansion at a lower dosage and has strong temperature resistance, and the temperature resistance can reach 220 DEG C.

Description

technical field [0001] The invention relates to a preparation method of an N-alkylated triamine-based star-shaped ultra-low molecular inhibitor used for inhibiting bentonite hydration and pulping during oil drilling. Background technique [0002] With the increase of exploration and development of oil and gas resources in deep formations, the drilling depth continues to increase, and the probability of encountering hydration-swelling clay minerals such as montmorillonite or illuminator / smectite layer increases accordingly, and the large well depth leads to a longer drilling fluid circulation time. However, the temperature in the middle and lower sections of deep wells is relatively high. Due to the long-term high temperature, it is difficult for the inhibitors in the drilling fluid system to stably inhibit the latter's hydration expansion and mud formation, resulting in unfavorable well conditions such as creep shrinkage and bit balling. Frequently, drilling operations are d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/24C07C211/14C09K8/035
Inventor 罗霄韩午丽任晗卢福伟
Owner YANGTZE UNIVERSITY
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