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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  • Summary
  • 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 tr

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
Comparison scheme
Effect test

Example Embodiment

[0037] Example 1

[0038] Synthesis of 0.5-generation polyamide-amine (PAMAM-0.5G): Put 15.3g (0.25mol) ethylenediamine, 40g ethanol, 0.15gBF into a 250ml four-necked 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 while stirring, and react for 12 hours under stirring at 25°C to obtain a light yellow liquid.

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

[0040]Synthesis of 1.5 generation polyamide-amine (PAMAM-1.5G): Add 63g of the previously synthesized PAMAM-1.0G, 50g of ethanol, and 0.10g of BF to a 250ml four-necked flask 3 ·Et 2 O, 43.5g methyl acrylate (0.5mol)...

Example Embodiment

[0042] Example 2

[0043] Synthesis of 0.5-generation polyamide-amine (PAMAM-0.5G): Add 17g (0.25mol) ammonia (25%), 50g methanol, 0.5g AlCl in a 100ml four-necked flask 3 , 65.2g (0.75mol) methyl acrylate was added dropwise and reacted for 8h under stirring conditions 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 transferred to a 500ml reaction flask without separation, 60g methanol is added, and 45.9g (0.75mol) ethylenediamine is added dropwise. React at 35°C for 8h under stirring conditions. A light yellow liquid is obtained.

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

[0046] S...

Example Embodiment

[0047] Example 3

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

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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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