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Method for preparing stellate poly quaternary ammonium salt high efficient reverse-phase emulsifier

A technology of inverse demulsifier and polyquaternary ammonium salt, which is used in immiscible liquid separation, flocculation/sedimentation water/sewage treatment, etc. It can solve the problem of increased difficulty in oil extraction sewage treatment, unsatisfactory performance, and types of inverse demulsifiers. Single problem, to achieve the effect of simple and easy synthesis process, mild synthesis conditions, and no three waste emissions

Active Publication Date: 2009-02-04
CHINA NAT OFFSHORE OIL CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, with the implementation of enhanced oil recovery technologies such as polymer flooding, steam flooding, surfactant flooding, alkali flooding, and deep profile control and water shutoff, the difficulty of oil production wastewater treatment is increasing. It has been unable to meet the needs of oil field development, mainly manifested in the single type of inverse demulsifier suitable for oil-in-water (o / w) emulsion of oil production sewage, and the performance is not ideal

Method used

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  • Method for preparing stellate poly quaternary ammonium salt high efficient reverse-phase emulsifier
  • Method for preparing stellate poly quaternary ammonium salt high efficient reverse-phase emulsifier
  • Method for preparing stellate poly quaternary ammonium salt high efficient reverse-phase emulsifier

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Synthesis of 0.5 generation polyamidoamine (PAMAM-0.5G): Add 15.3g (0.25mol) ethylenediamine, 40g ethanol, 0.15gBF to a 250ml four-neck flask 3 ·Et 2 O, add 86.9 (1.0 mol) methyl acrylate dropwise at a constant rate of 1.5 to 2 hours at a temperature of 20-25°C under stirring, and react for 12 hours under stirring at 25°C to obtain a light yellow liquid.

[0039] Synthesis of 1.0th generation polyamide-amine (PAMAM-1.0G): without separation of the 0.5th generation product synthesized above, add 50g of ethanol, stir and control the temperature at 20-25°C, continue to drop 61.2g (1.0mol) ethylene glycol The amine was added in 1.5~2h, and then reacted at 25°C for 12h while stirring. A pale yellow liquid was obtained.

[0040]Synthesis of 1.5 generation polyamide-amine (PAMAM-1.5G): add 63g of PAMAM-1.0G synthesized earlier, 50g of ethanol, 0.10g of BF in a 250ml four-neck flask 3 ·Et 2 O, 43.5 g of methyl acrylate (0.5 mol) was added dropwise, and reacted for 12 h unde...

Embodiment 2

[0043] Synthesis of 0.5 generation polyamido-amine (PAMAM-0.5G): Add 17g (0.25mol) ammonia water (25%), 50g methanol, 0.5gAlCl to a 100ml four-necked flask 3 , 65.2g (0.75mol) of methyl acrylate was added dropwise, and reacted for 8h under stirring at 30°C to obtain a light yellow liquid.

[0044] Synthesis of 1.0 generation polyamide-amine (PAMAM-1.0G): The 0.5 generation product synthesized above is not separated, transferred to a 500ml reaction bottle, added 60g methanol, and continued to drop 45.9g (0.75mol) ethylenediamine, in The reaction was carried out at 35°C for 8h with stirring. A pale yellow liquid was obtained.

[0045] Synthesis of 1.5 generation polyamide-amine (PAMAM-1.5G): add 119g of previously synthesized PAMAM-1.0G, 50g methanol, 0.5g AlCl to a 250ml four-necked flask 3 , 65.2 g of methyl acrylate (0.75 mol) was added dropwise, and reacted for 8 h under stirring at 30° C. to obtain a light yellow liquid.

[0046] Synthesis of 2.0-generation polyamide-ami...

Embodiment 3

[0048] Synthesis of linear polyquaternium (LPQA): add 89.6 g (0.4 mol) of dodecyl tertiary amine in a 2L four-necked reaction flask equipped with a reflux condenser, add 45 g (0.44 mol) of concentrated hydrochloric acid dropwise at room temperature, and then add 100g of methanol, 40.7g of epichlorohydrin (0.44mol) was added dropwise at 40°C, after the addition was completed, the reaction was kept at 55°C for 3h, then 436.5g (3.2mol) of dimethylamine (33%) was added, and 297.6g of dimethylamine (33%) was added dropwise at room temperature Add epichlorohydrin (3.2 mol) for about 1 hour. After the addition, keep the temperature at 40°C for 1 hour, then raise the temperature to 105°C for 1 hour, add 526g of water, and mix well to obtain the product.

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Abstract

The invention provides a method for preparing a high efficiency antiphase demulsifying agent of astroid poly (quaternary ammonium salt), which belongs to the technical field of water curing. Firstly, linear poly (quaternary ammonium salt) is prepared with organic amines such as secondary amine and tertiary amine together with epichlorohydrin through ring-expansion polymerization; subsequently, PAMAM is used as a cross-linking agent, thus getting the antiphase demulsifying agent. The antiphase demulsifying agent is characterized in that the reaction conditions are gentle; raw materials are available; the product structure is unique; the antiphase demulsifying agent contains cationic organic polymer macromolecules, which has the properties of electric neutralization, substitution, absorption and bridging; such pollutants as oil and suspended matter in oil-contaminated water can be effectively removed by adding 5 to 30ppm of the antiphase demulsifying agent; such indices as oil content, colour shade, COD and so on in polluted water to be polluted are effectively reduced.

Description

technical field [0001] The invention relates to the field of oily sewage treatment produced in industries such as oil extraction, refining, steel rolling and the like, and relates to a preparation method of a star-shaped polyquaternium high-efficiency reverse-phase demulsifier. Background technique [0002] With the rapid development of industry, the amount of oily wastewater produced in oilfield mining, refining, ink, steel and other industries is increasing. The wide application of various surfactants increases the stability of oily emulsions and makes their treatment more difficult. Large, the existing inverse demulsifier for oily sewage treatment can no longer meet the production needs. In particular, some oilfields are currently entering a period of high water-cut development, and the oil-water ratio in the produced fluid has dropped sharply. The comprehensive water content of many oilfields has reached more than 90%, and the amount of oil production wastewater to be tr...

Claims

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Application Information

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IPC IPC(8): C08G73/00B01D17/04C02F1/56
Inventor 王素芳姚光源林蓓李家俊滕厚开郑书忠
Owner CHINA NAT OFFSHORE OIL CORP
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