A kind of preparation method of branched polyethyleneimine and shale intercalation inhibitor

A technology of branched polyethyleneimine and polyethylene polyamine, which is applied in the field of oil and gas field drilling, and achieves the effects of high yield, good water solubility and low price

Active Publication Date: 2020-02-11
SOUTHWEST PETROLEUM UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Another object of the present invention is to provide a shale intercalation inhibitor configured by branched polyethyleneimine to solve the problem of intercalation inhibiting clay mineral surface hydration

Method used

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  • A kind of preparation method of branched polyethyleneimine and shale intercalation inhibitor
  • A kind of preparation method of branched polyethyleneimine and shale intercalation inhibitor
  • A kind of preparation method of branched polyethyleneimine and shale intercalation inhibitor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] The synthetic steps (step S1) of aziridine are as follows:

[0049] In a low-temperature reaction vessel at 15°C, react ethanolamine with a molar ratio of 1:1.1 and concentrated sulfuric acid:

[0050] S11. First, dissolve 0.5mol ethanolamine in 80ml of toluene, slowly add 32mL of 95% concentrated sulfuric acid dropwise while stirring at low temperature, and drop the concentrated sulfuric acid within 15 minutes; continue stirring for 30 minutes after the dropwise addition, and distill under reduced pressure. When the volume of the mixed system was concentrated to 1 / 4 of the original volume, the temperature was raised to 180° C. until no moisture was evaporated to solidify the material, and the reaction was stopped after heating at 180° C. for 1 h to obtain 69.2 g of solid powder β-aminoethyl sulfate. Productive rate reaches 98%; S12, when the temperature of β-aminoethylsulfate drops to 10 DEG C, slowly add 250g of 40% by mass NaOH solution, heat and stir simultaneously,...

Embodiment 2

[0054] The aziridine and diethylenetriamine prepared by embodiment 1 are used as raw materials, and branched polyethyleneimine is prepared by step-by-step synthesis, and the specific steps are as follows:

[0055] (1) Synthesis of G1 branched polyethyleneimine: Dissolve 0.1mol diethylenetriamine in absolute ethanol, add 0.5mol ethanol solution of aziridine dropwise at 50°C, after the dropwise addition, heat Reflux reaction for 6h, and then vacuum distillation to obtain G1 branched polyethyleneimine with a yield of 97.4%. Molecular formula of G1 branched polyethyleneimine: C 14 h 38 N 8 , exact molecular weight: 318.3219, molar mass: 318.5140, mass-to-charge ratio: 318.322 (100.00%), 319.325 (15.1%), 320.329 (1.1%). Elemental analysis: C, 52.79; H, 12.03; N, 35.18. Such as figure 2 As shown, the mass-to-charge ratio measured by LC-MS is 319.329, because the G1 branched polyethyleneimine obtains a proton, and its molecular weight of 318.329 is consistent with the theoretic...

Embodiment 3

[0062] Aziridine and diethylenetriamine prepared in Example 1 are used as raw materials, and branched polyethyleneimine is prepared by a one-pot synthesis method, and the specific steps are as follows:

[0063] Dissolve 0.1mol diethylenetriamine in absolute ethanol, add 3.5mol ethanol solution of aziridine compound dropwise at 50°C, after the dropwise addition, reflux for 12 hours, and then distill under reduced pressure to obtain a wide molecular weight distribution The G4 branched polyethyleneimine, the yield is 92.6%. From the mass spectrum ( Figure 5 ), it can be seen that the molecular weight distribution of the branched polyethyleneimine synthesized by the one-pot method is relatively wide, indicating that the G4 branched polyethyleneimine has a variety of molecular structures, including not only the G1 branched polyethyleneimine prepared in Example 2 Amine and G2 branched polyethyleneimine also mainly have the following molecular structural formula:

[0064]

[00...

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Abstract

The invention discloses a preparation method of branched polyethyleneimine and a shale intercalation inhibitor prepared from the branched polyethyleneimine. The branched polyethyleneimine is preparedby the following steps: S1. synthesizing aziridine; S2. with a polyamine compound and the aziridine as raw materials, preparing the branched polyethyleneimine by a stepwise synthesis process or a one-pot synthesis process, wherein the polyamine compound is polyethylene polyamine or alkylamine; the polyethylene polyamine is one of diethylenetriamine, triethylene tetramine, tetraethylenepentamine and pentaethylenehexamine; the alkylamine is one of ethylenediamine, propane diamine, butanediamine, pentamethylene diamine, nonamethylene diamine and decamethylene diamine. The shale intercalation inhibitor is prepared by proportionally mixing the branched polyethyleneimine with water. The branched polyethyleneimine synthesis method provided by the invention has the advantages of high yield and cheap raw materials and is suitable for large-scale industrial production; the shale intercalation inhibitor prepared from the branched polyethyleneimine can effectively alleviate the problem of unstableborehole wall caused by the hydration dispersion of shale.

Description

technical field [0001] The invention belongs to the technical field of oil and gas field drilling, and in particular relates to a synthesis method of low-molecular-weight branched polyethyleneimine suitable for complex shale drilling and a shale intercalation inhibitor prepared by using branched polyethyleneimine. Background technique [0002] Well wall instability often leads to downhole complex accidents such as well wall collapse, diameter shrinkage, and pipe sticking, which increases drilling time and drilling costs. 75% of wellbore instability mainly occurs in shale formations, especially water-sensitive formations. Oil-based drilling fluid has the advantages of good wellbore stability and strong suppression ability, but there are problems such as serious environmental pollution, difficult disposal, and high disposal cost. Therefore, it is a trend in the development of drilling fluid technology to develop water-based drilling fluids with the same effect as oil-based dr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/02
CPCC08G73/0206C08G73/0213C09K8/035C09K2208/12
Inventor 谢刚罗平亚邓明毅黄丹超马玉玲王宇
Owner SOUTHWEST PETROLEUM UNIV
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