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Hyperbranched small molecular intercalation agent with primary amine group as the terminal group and preparation method thereof

A primary amine group, small molecule technology, applied in the field of hyperbranched small molecule intercalating agents and their preparation, can solve problems such as the difficulty of maintaining the adsorption form of intercalating agent molecules, limiting the inhibition efficiency of the intercalating agent, and the limited inhibition efficiency. , to achieve the effect of controllable molecular size and structure, inhibition of hydration expansion and dispersion migration, and low cost

Inactive Publication Date: 2019-07-12
YANGTZE UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing amine-based intercalants are mostly flexible linear small molecules, and their adsorption morphology in the clay interlayer domain is mainly ring-type and horizontal-type, which occupy a small space and volume, and the protonated groups located at both ends of the molecule The clusters are all adsorbed on the surface of the same crystal layer. When the drilling fluid penetrates into the formation due to the pressure difference, it is difficult for the intercalation agent molecules to maintain a firm adsorption state, and its inhibitory effect is limited. The molecular thermal motion of the molecule is aggravated by heat, and the probability of desorption increases, which further limits the inhibitory performance of the intercalation agent.

Method used

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  • Hyperbranched small molecular intercalation agent with primary amine group as the terminal group and preparation method thereof
  • Hyperbranched small molecular intercalation agent with primary amine group as the terminal group and preparation method thereof
  • Hyperbranched small molecular intercalation agent with primary amine group as the terminal group and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 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.

[0029] 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

[0033] This example is a preparation example of 1,1,1-triformaldehyde propane.

[0034] 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 1,1,1-trimethylolpropane dropwise to the three-necked flask under stirring at room temperature to ensure that the molar ratio of the hydroxyl group of 1,1,1-trimethylolpropane to the PCC reagent is 1:1.5 , After the dropwise addition, the reaction was continued for 4h and then the reaction was stopped. Pour out the upper layer solution, the lower layer of solid matter was washed 3 times with DCM, the upper layer solution and the washing liquid were combined, and the combined solution was successively washed with saturated NaHCO 3 Washed with aqueous solution, followed by anhydrous Na 2 SO 4 After drying and filteri...

Embodiment 3

[0040] This example is a preparation example of 1,1,1-triaminomethylpropane.

[0041] 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-triformylpropane 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, which was filtered under reduced pressure to remove the black coke impurities, and the obtained filtrate was successively washed with saturated NaHCO 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 4The upper mother liquor...

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Abstract

The invention discloses a hyperbranched small molecular intercalation agent with a primary amine group as the terminal group and a preparation method thereof. The molecular structure of the hyperbranched small molecular intercalation agent is as shown in the specification. The hyperbranched small molecular intercalation agent is prepared by using 1,1,1-trimethylolpropane as the raw material and successively through an oxidation reaction and a Leuckart-Wallach reaction. The hyperbranched small molecular intercalation agent has characteristics of controllable molecular dimension and structure, high terminal protonated group density and uniform space distribution, has strong inhibition performance on both hydration pulping effect of bentonite and mud shale, can effectively inhibit hydration swelling and dispersion migration of bentonite and mud shale, and has good temperature-tolerance performance. The temperature-tolerance performance can reach 150 DEG C.

Description

technical field [0001] The invention belongs to the technical field of petroleum drilling, and particularly relates to a hyperbranched small molecule intercalation agent whose end group is a primary amine group and a preparation method thereof. The hyperbranched small molecule intercalation agent is used for inhibiting bentonite and Slurry of mud shale. Background technique [0002] With the gradual increase in the exploration and development of oil and gas resources in deep formations, the circulation time of the drilling fluid system is greatly prolonged. If the system cannot effectively inhibit the expansion and slurry formation of clay minerals in the downhole slurry, it will cause creep shrinkage and Unfavorable well conditions such as bit balling. In addition, the temperature in the middle and lower sections of deep wells and ultra-deep wells is high, and the inhibitors in the system are prone to decline in inhibitory performance due to long-term high temperature effe...

Claims

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Application Information

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IPC IPC(8): C07C209/28C07C211/13C07C45/29C07C47/02C09K8/035C09K8/22
CPCC07C45/29C07C209/28C07C211/13C09K8/035C09K8/22C09K2208/12C07C47/02
Inventor 罗霄任晗韩午丽卢福伟
Owner YANGTZE UNIVERSITY
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