CN102234374A - Method for preparing dendrimer antiphase demulsifier - Google Patents
Method for preparing dendrimer antiphase demulsifier Download PDFInfo
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- CN102234374A CN102234374A CN 201010166695 CN201010166695A CN102234374A CN 102234374 A CN102234374 A CN 102234374A CN 201010166695 CN201010166695 CN 201010166695 CN 201010166695 A CN201010166695 A CN 201010166695A CN 102234374 A CN102234374 A CN 102234374A
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Abstract
The invention discloses a method for preparing a dendrimer antiphase demulsifier used for demulsifying crude oil. Based on the total weight, 0.1 to 10 percent of 1.0 generation, 2.0 generation and 3.0 generation dendrimer polyamide-amine, 10 to 45 percent of epoxy chloropropane, and 5 to 22 percent of dimethylamine form an aqueous solution containing 10 to 40 percent of the composition at different concentrations. The method comprises the following steps of: synthesizing the 1.0 generation, 2.0 generation and 3.0 generation dendrimer polyamide-amine; taking 1.0 generation dendrimer polyamide-amine, 2.0 generation dendrimer polyamide-amine and 3.0 generation dendrimer polyamide-amine in different ratios, adding a proper amount of epoxy chloropropane at the temperature of below 40DEG C, reacting for 2 to 4 hours, adding a certain amount of dimethylamine, dripping epoxy chloropropane accounting for 90 percent of the total addition amount into the mixed solution, heating to the temperature of between 85 and 95DEG C, reacting for 1 hour; and adding the rest 10 percent of epoxy chloropropane by three times at time intervals of 20 minutes, and keeping the temperature of between 85 and 95DEG C until the reaction is fully carried out.
Description
Technical field
The present invention is a kind of preparation method of dendroid reverse-phase emulsifier of crude oil demulsification.Relate to the petroleum industry technical field.
Background technology
Along with the use of the fast development in oil field and a large amount of electric submersible pump, the oil field is adopted liquid measure and is increased the raising of water content.Because the speed that electric submersible pump is high is sheared, the emulsification of crude oil in water is serious, has increased the turbidity of dehydrating of crude oil, to the demands for higher performance of reverse-phase emulsifier.Reverse-phase emulsifier commonly used has bodied ferric sulfate, polymerize aluminum chloride, polyacrylamide, ammonia-epoxy chloropropane polycondensate and ammonia-dimethylamine-epichlorohydrin polymer etc., and the follow-up people of having is used for crude oil demulsification with the polyamide-amide branch-shape polymer.Effect and the effect of dissimilar reverse-phase emulsifiers in oilfield sewage rp demulsification process has notable difference, and generally showing as inorganic polymer, to have a de-emulsification speed fast, but add-on is big, and it is little to have add-on for linear organic polymer, but the treatment time is long.The colinearity polymkeric substance improves breakdown of emulsion efficient to than, the emulsification interface of the easier destruction profit of branch-shape polymer.
Summary of the invention
The preparation method who the objective of the invention is to invent a kind of rapid damage oil-water emulsion interface, improve breakdown of emulsion efficient, the dendroid reverse-phase emulsifier of back water quality is handled in raising.
The present invention is made up of dendroid polyamide-amide (PAMAM), epoxy chloropropane, the dimethylamine in 1.0 generations to 3.0 generations; Its proportioning is: in gross weight is in 100, and the dendroid polyamide-amide (PAMAM) in 1.0 generations to 3.0 generations accounts for 0.1%-10%, and epoxy chloropropane accounts for 10-45%, dimethylamine accounts for 5%-22%, forms to contain the above-mentioned synthetics solution in different concentration of 10%-40%.
The preparation method of this dendroid reverse-phase emulsifier:
The dendroid polyamide-amide (PAMAM) at first synthetic 1.0 generations to 3.0 generations;
Reaction comprises two processes: the one, and quadrol and methyl acrylate carry out the Michael addition reaction, the polynary ester that reaction obtains, carry out amidate action again with quadrol and obtain acid amides, thereby obtain the macromole branch-shape polymer: polyamide-amide by hocket Michael addition and amidate action; The dendroid polyamide-amide in synthetic 1.0 generations, 2.0 generations and 3.0 generations needs earlier synthetic 0.5 generation;
0.5 synthetic for PAMAM: having agitator, thermometer adds quadrol in the four-hole boiling flask of prolong, methyl alcohol, controlled temperature is at 20 ℃-30 ℃, turn on agitator, slowly add methyl acrylate, be controlled in two hours and add continuation reaction about 16 hours-24 hours; After reaction was finished, it was 20 ℃-30 ℃ that temperature is set in vacuum drying oven, and vacuum tightness vacuumizes for the 1mmHg post, and unnecessary reactant and solvent are drained, and obtains the PAMAM that flaxen product was for 0.5 generation at last;
1.0 synthetic for PAMAM: add quadrol and methyl alcohol in four-hole boiling flask, the methanol solution of synthetic 0.5 generation PAMAM maintains the temperature at 20 ℃-30 ℃ above slowly dripping, and reacts 36 hours-48 hours; After reaction finished, it was 65 ℃-75 ℃ that temperature is set in vacuum drying oven, and vacuum tightness vapors away unnecessary quadrol and methyl alcohol for the 2mmHg post vacuumizes, and obtains flaxen product and is 1.0 generation PAMAM;
Hocket Michael addition and amidate action can obtain for 1.5 generations, 2.0 generations, 2.5 generations, 3.0 generation PAMAM;
1.0 generations, 2.0 generations and the 3.0 generation PAMAM that get different ratios are lower than 40 ℃ in temperature and added an amount of epichlorohydrin reaction 2 hours-4 hours down, add a certain amount of dimethylamine, drip the epoxy chloropropane that accounts for total add-on 90% to miscible fluid, temperature is increased to 85 ℃-95 ℃, reacts 1 hour; Described 1.0 generations, 2.0 generations and 3.0 generation PAMAM ratio in polymkeric substance can be single component, two-pack and three components; For two-pack, the ratio of two components is 1: 4,2: 3, and 1: 1; For three components, each ratio can be 1: 1: 1, and 1: 2: 2,1: 2: 3,1: 2: 4 etc.;
Branch will remain 10% epoxy chloropropane adding several times again, and in each 20 minutes timed intervals that add, temperature keeps 85 ℃-95 ℃, to reacting completely.
The present invention is the reverse-phase emulsifier that is used for the field produces sewage disposal, this reverse-phase emulsifier is compared with existing reverse-phase emulsifier, have following difference: this reverse-phase emulsifier is that the dendroid polyamide-amide with 1.0 generations to 3.0 generations is the nuclear of branch, and then add epoxy chloropropane and dimethylamine reacts, branch is gone up be dimethylamine-epichlorohydrin polymer.Breakdown of emulsion efficient is improved at emulsification interface that can the rapid damage profit, improves the water quality after handling.
Embodiment
Embodiment. this example is made up of dendroid polyamide-amide (PAMAM), epoxy chloropropane, dimethylamine, the epoxy chloropropane in 1.0 generations to 3.0 generations; Its proportioning is: in gross weight is in 100, and the dendroid polyamide-amide (PAMAM) in 1.0 generations to 3.0 generations accounts for 8%, and epoxy chloropropane accounts for 35%, dimethylamine accounts for 15%, forms the aqueous solution that contains 58% above-mentioned synthetics.
The preparation method of this dendroid reverse-phase emulsifier:
The dendroid polyamide-amide (PAMAM) at first synthetic 1.0 generations to 3.0 generations;
Reaction comprises two processes: the one, and quadrol and methyl acrylate carry out the Michael addition reaction, the polynary ester that reaction obtains, carry out amidate action again with quadrol and obtain acid amides, thereby obtain the macromole branch-shape polymer: polyamide-amide by hocket Michael addition and amidate action; The dendroid polyamide-amide in synthetic 1.0 generations, 2.0 generations and 3.0 generations needs earlier synthetic 0.5 generation;
0.5 synthetic for PAMAM: having agitator, thermometer adds the 4g quadrol in the four-hole boiling flask of prolong, 30ml methyl alcohol, controlled temperature is at 25 ℃, turn on agitator, slowly add the 50g methyl acrylate, be controlled in two hours and add about 20 hours of continuation reaction; After reaction was finished, it was 25 ℃ that temperature is set in vacuum drying oven, and vacuum tightness vacuumizes for the 1mmHg post, and unnecessary reactant and solvent are drained, and obtains the PAMAM that flaxen product was for 0.5 generation at last;
1.0 synthetic for PAMAM: add 60g quadrol and methyl alcohol in four-hole boiling flask, the methanol solution of synthetic 0.5 generation PAMAM maintains the temperature at 25 ℃ above slowly dripping, and reacts 40 hours; After reaction finished, it was 70 ℃ that temperature is set in vacuum drying oven, and vacuum tightness vapors away unnecessary quadrol and methyl alcohol for the 2mmHg post vacuumizes, and obtains flaxen product and is 1.0 generation PAMAM;
Hocket Michael addition and amidate action can obtain for 1.5 generations, 2.0 generations, 2.5 generations, 3.0 generation PAMAM;
1.0 generations, 2.0 generations and the 3.0 generation PAMAM that get different ratios are lower than 40 ℃ of epichlorohydrin reactions that add 20g down 2 hours in temperature, the dimethylamine that adds 80g, drip 150g epoxy chloropropane (90% of total add-on to miscible fluid, add continuously, the speed that adds is controlled according to heat of reaction, guarantee that temperature of reaction is lower than 40 ℃), temperature is increased to 85 ℃, reacts 1 hour; Divide the epoxy chloropropane that falls residue 10% for three times again, in each 20 minutes timed intervals that add, temperature keeps 85 ℃, to reacting completely.
Is that the sewage of 3300NUT is seen the row test with the dendroid reverse-phase emulsifier of this preparation method preparation for the Sudan's 1/2/4 oil field turbidity, and adding dosage is 10ppm, the sewage turbidity can be reduced to less than 50NUT.
Application conditions: the sewage disposal that oil field CPF and FPF treatment station are deviate from.
The form of product: the product water soluble can be made into the product that concentration is 10%-40%.
The dendroid reverse-phase emulsifier of present method preparation can the rapid damage profit the emulsification interface, improve breakdown of emulsion efficient, improve the water quality after handling.
Claims (3)
1. the preparation method of the dendroid reverse-phase emulsifier of a crude oil demulsification is characterized in that being made up of dendroid polyamide-amide, epoxy chloropropane, the dimethylamine in 1.0 generations to 3.0 generations; Its proportioning is: in gross weight is in 100, and the dendroid polyamide-amide in 1.0 generations to 3.0 generations accounts for 0.1%-10%, and epoxy chloropropane accounts for 10-45%, dimethylamine accounts for 5%-22%, forms to contain the above-mentioned synthetics solution in different concentration of 10%-40%;
The dendroid polyamide-amide at first synthetic 1.0 generations to 3.0 generations; Get different ratios 1.0 generations, 2.0 generations and 3.0 generation the dendroid polyamide-amide be lower than 40 ℃ in temperature and added an amount of epichlorohydrin reaction 2 hours-4 hours down, add a certain amount of dimethylamine, drip the epoxy chloropropane that accounts for total add-on 90% to miscible fluid, temperature is increased to 85 ℃-95 ℃, reacts 1 hour; Divide will remain 10% epoxy chloropropane for three times and add, in each 20 minutes timed intervals that add, temperature keeps 85 ℃-95 ℃, to reacting completely again.
2. the preparation method of a kind of dendroid reverse-phase emulsifier according to claim 1, the dendroid polyamide-amide that it is characterized in that described synthetic 1.0 generations to 3.0 generations is that its reaction comprises two processes: the one, and quadrol and methyl acrylate carry out the Michael addition reaction, the polynary ester that reaction obtains, carry out amidate action again with quadrol and obtain acid amides, thereby obtain the macromole branch-shape polymer: polyamide-amide by hocket Michael addition and amidate action;
The dendroid polyamide-amide in synthetic 1.0 generations, 2.0 generations and 3.0 generations needs earlier synthetic 0.5 generation;
0.5 synthetic for PAMAM: having agitator, thermometer adds quadrol in the four-hole boiling flask of prolong, methyl alcohol, controlled temperature is at 20 ℃-30 ℃, turn on agitator, slowly add methyl acrylate, be controlled in two hours and add continuation reaction about 16 hours-24 hours; After reaction was finished, it was 20 ℃-30 ℃ that temperature is set in vacuum drying oven, and vacuum tightness vacuumizes for the 1mmHg post, and unnecessary reactant and solvent are drained, and obtains the PAMAM that flaxen product was for 0.5 generation at last;
1.0 synthetic for PAMAM: add quadrol and methyl alcohol in four-hole boiling flask, the methanol solution of synthetic 0.5 generation PAMAM maintains the temperature at 20 ℃-30 ℃ above slowly dripping, and reacts 36 hours-48 hours; After reaction finished, it was 65 ℃-75 ℃ that temperature is set in vacuum drying oven, and vacuum tightness vapors away unnecessary quadrol and methyl alcohol for the 2mmHg post vacuumizes, and obtains flaxen product and is 1.0 generation PAMAM;
Hocket Michael addition and amidate action can obtain for 1.5 generations, 2.0 generations, 2.5 generations, 3.0 generation PAMAM.
3. the preparation method of dendroid reverse-phase emulsifier according to claim 1 is characterized in that described 1.0 generations, 2.0 generations and 3.0 generation PAMAM ratio in polymkeric substance, is single component, two-pack or three components; For two-pack, the ratio of two components is 1: 4,2: 3, and 1: 1; For three components, each ratio can be 1: 1: 1, and 1: 2: 2,1: 2: 3,1: 2: 4.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102233249A (en) * | 2010-04-30 | 2011-11-09 | 中国石油天然气集团公司 | Dendritic reverse demulsifier and preparation method thereof |
| CN102559246A (en) * | 2012-02-16 | 2012-07-11 | 中国海洋石油总公司 | Reverse demulsifier and its preparation method |
| CN102559245A (en) * | 2012-02-16 | 2012-07-11 | 中国海洋石油总公司 | Reverse demulsifier and preparation method thereof |
| US9475894B2 (en) | 2013-06-25 | 2016-10-25 | China Petroleum & Chemical Corporation | Dendritic polymer, dendritic polymer monomer, and hyperbranched copolymer |
| CN108192096A (en) * | 2017-12-15 | 2018-06-22 | 中国海洋石油集团有限公司 | A kind of preparation method of modified dendritic interphase reverse-phase emulsifier |
| CN110105546A (en) * | 2019-06-10 | 2019-08-09 | 威海晨源分子新材料有限公司 | Epoxy curing agent, preparation method and application |
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| US4614593A (en) * | 1985-03-28 | 1986-09-30 | Ethyl Corporation | Demulsification of oil-in-water emulsions |
| CN101357992A (en) * | 2008-06-20 | 2009-02-04 | 中国海洋石油总公司 | Method for preparing stellate poly quaternary ammonium salt high efficient reverse-phase emulsifier |
| CN102233249A (en) * | 2010-04-30 | 2011-11-09 | 中国石油天然气集团公司 | Dendritic reverse demulsifier and preparation method thereof |
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2010
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Patent Citations (4)
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| US4568737A (en) * | 1983-01-07 | 1986-02-04 | The Dow Chemical Company | Dense star polymers and dendrimers |
| US4614593A (en) * | 1985-03-28 | 1986-09-30 | Ethyl Corporation | Demulsification of oil-in-water emulsions |
| CN101357992A (en) * | 2008-06-20 | 2009-02-04 | 中国海洋石油总公司 | Method for preparing stellate poly quaternary ammonium salt high efficient reverse-phase emulsifier |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102233249A (en) * | 2010-04-30 | 2011-11-09 | 中国石油天然气集团公司 | Dendritic reverse demulsifier and preparation method thereof |
| CN102559246A (en) * | 2012-02-16 | 2012-07-11 | 中国海洋石油总公司 | Reverse demulsifier and its preparation method |
| CN102559245A (en) * | 2012-02-16 | 2012-07-11 | 中国海洋石油总公司 | Reverse demulsifier and preparation method thereof |
| US9475894B2 (en) | 2013-06-25 | 2016-10-25 | China Petroleum & Chemical Corporation | Dendritic polymer, dendritic polymer monomer, and hyperbranched copolymer |
| US10047200B2 (en) | 2013-06-25 | 2018-08-14 | China Petroleum & Chemical Corporation | Dendritic polymer, dendritic polymer monomer, and hyperbranched copolymer |
| CN108192096A (en) * | 2017-12-15 | 2018-06-22 | 中国海洋石油集团有限公司 | A kind of preparation method of modified dendritic interphase reverse-phase emulsifier |
| CN108192096B (en) * | 2017-12-15 | 2020-09-29 | 中国海洋石油集团有限公司 | Preparation method of modified dendritic polyamide-amine reverse demulsifier |
| CN110105546A (en) * | 2019-06-10 | 2019-08-09 | 威海晨源分子新材料有限公司 | Epoxy curing agent, preparation method and application |
| CN110105546B (en) * | 2019-06-10 | 2022-02-08 | 威海晨源分子新材料有限公司 | Epoxy resin curing agent, preparation method and application thereof |
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Application publication date: 20111109 |