CN102942956B - Organic silicon resin grafted crude oil demulsification agent and preparation method thereof - Google Patents
Organic silicon resin grafted crude oil demulsification agent and preparation method thereof Download PDFInfo
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- CN102942956B CN102942956B CN201210508023.4A CN201210508023A CN102942956B CN 102942956 B CN102942956 B CN 102942956B CN 201210508023 A CN201210508023 A CN 201210508023A CN 102942956 B CN102942956 B CN 102942956B
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- silicone resin
- crude oil
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- oil demulsifier
- demulsification agent
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Abstract
The invention relates to an organic silicon resin grafted crude oil demulsification agent and a preparation method thereof. The preparation method of the organic silicon resin grafted crude oil demulsification agent comprises the following steps: (1) adding organic silicon resin, alkyl phenol and formaldehyde or formaldehyde water solution into a reaction kettle, heating to 80-90 DEG C, performing synthetic reaction, and then cooling to 60 DEG C or below; and (2) adding a strong alkali catalyst into the reaction product obtained in the step (1), introducing epoxyethane and epoxypropane, heating to 120-130 DEG C, performing synthetic reaction, then cooling, and discharging. The technical scheme of the invention has the following main advantages: (1) the raw materials are resistant to high temperature and low temperature, thereby being beneficial to improving the high-temperature and low-temperature stability of the demulsification agent; (2) the raw materials are low in viscosity and can be mixed quickly, thereby shortening the demulsification time; (3) the demulsification agent is low in surface energy and can be easily mixed with crude oil; (4) the demulsification agent is wide in application range and is applicable to various types of crude oil; and (5) the demulsification agent has the characteristics of favorable effect, high dehydration speed and less consumption.
Description
(1) technical field
The invention belongs to a kind of production method of silicone resin modification nonionogenic tenside, particularly a kind of silicone resin grafting crude oil demulsifier and preparation method thereof.
(2) background technology
Crude oil exists with milk sap in extraction process, and dehydration is one of important step in petroleum production processes process.At present, the most frequently used reason breaking method of petroleum industry adds emulsion splitter in crude oil, and crude oil in China component is comparatively complicated, different geographical, different blocks, also there is different difference in even not same oil well oil, and emulsion splitter has stronger specific aim, which increase the use difficulty of emulsion splitter.Along with the development of China's tertiary oil recovery technology, the composition of crude oil Produced Liquid becomes increasingly complex, and also worse and worse, this type of crude oil demulsification difficulty is increasing, and breakdown of emulsion temperature constantly raises, and the scope of application is more and more narrow for stability, can not meeting the market requirement.
(3) summary of the invention
The present invention adopts modern biotechnology fermentation technique, provides a kind of high-low temperature resistant, applied widely, effective silicone resin grafting crude oil demulsifier and preparation method thereof.
The present invention is achieved through the following technical solutions:
A kind of silicone resin grafting crude oil demulsifier, its special character is: be made up of the raw material of following parts by weight:
Silicone resin 5-10 part
Alkylphenol 10-15 part
Oxyethane 15-20 part
Propylene oxide 30-45 part
Highly basic 1-5 part
Platinic chloride 0.05-0.1 part
Formaldehyde 9-11 part or
The formalin of equal quality.
The reaction of its corresponding chemical is:
Wherein R is alkyl, and Ph is phenyl, and Y is modified phenolic resins, and Xc is silicone resin, [X
c]-[Y] be silicone resin graft resin, Po is oxyethane, and PE is propylene oxide, A, B for link number, A is the integer in 15-20, and B is the integer in 30-45, and Platinic chloride and highly basic are catalyzer.
Silicone resin grafting crude oil demulsifier of the present invention, silicone resin be phenyl official can silicone resin, polyether type organic silicone resin, the silicone resin of amino-functional, at least one of hydrogeneous silicone resin, alkylphenol be base phenol, heptyl phenol, octyl phenol, nonyl phenol, certain herbaceous plants with big flowers base phenol one or more.
Silicone resin grafting crude oil demulsifier of the present invention, preferred formalin in raw material formaldehyde and formalin, containing formaldehyde 9-11 part in formalin, preferably, the mass percentage concentration of formalin is 37%, and addition is 25-30 part.
The preparation method of silicone resin grafting crude oil demulsifier of the present invention, its special character is: comprise the following steps: the synthesis of (1) silicone resin graft resin: by silicone resin, alkylphenol, formaldehyde or formalin and catalyzer Platinic chloride, add in reactor, be warming up to 80-90 DEG C and carry out building-up reactions, be then cooled to less than 60 DEG C;
(2) synthesis of emulsion splitter: step (1) gained reactant is added alkali catalyst, passes into oxyethane and propylene oxide, intensification 120-130 DEG C is carried out building-up reactions, blowing of then lowering the temperature.
The preparation method of silicone resin grafting crude oil demulsifier of the present invention, adds formalin in step (1), carries out processed after building-up reactions.
The preparation method of silicone resin grafting crude oil demulsifier of the present invention, in step (2), highly basic is potassium hydroxide.
Technical scheme of the present invention, its major advantage is as follows:
(1) high temperature resistant, be conducive to emulsion splitter higher than the stability under 150 DEG C of high temperature;
(2) viscosity is low, is about 0.606mpas and mixes fast, decreasing the breakdown of emulsion time;
(3) surface energy is low, is about 22.5mN/m, easily mixes with crude oil;
(4) applied widely, be applicable to all kinds crude oil;
(5) effective, dehydration is fast, consumption is few, mixing 5min gets final product layering.
(4) embodiment
Embodiment 1:
(1), the synthesis of silicone resin grafting:
By silicone resin 60kg, nonyl phenol 130 kg, formaldehyde (mass percentage concentration is 37%) 250 kg, Platinic chloride 0.5 kg of phenyl official energy, add in reactor, be warmed up to 80 DEG C, keep temperature 80-90 DEG C, reaction 3h, vacuum hydro-extraction 157.5 kg, be cooled to 60 DEG C stand-by.
(2), the synthesis of emulsion splitter:
By front step silicone resin graft resin, hydro-oxidation potassium 10 kg, be warmed up to 120 DEG C-130 DEG C, then pass into oxyethane 150 kg, propylene oxide 400 kg, reaction 2-3h, cooling blowing.
Corresponding chemical formula is:
Wherein R is C
9h
19-, Ph is phenyl, and Y is modified phenolic resins, [X
c]-[Y] be silicone resin graft resin, Po is oxyethane, and PE is propylene oxide, A, B for link number, A is 15, B is 40, silicone resin Xc be phenyl official can silicone resin, structural formula is
Link number m, n be greater than 0 integer, Platinic chloride and potassium hydroxide are catalyzer.
Embodiment 2:
(1), the synthesis of silicone resin grafting tree:
By polyether type organic silicone resin 80 kg, octyl phenol 120 kg, formaldehyde (mass percentage concentration is 37%) 220 kg, Platinic chloride 0. 6 kg join in reactor, are warmed up to 80 DEG C, sustaining temperature 80-90 DEG C, reaction 4h, vacuum hydro-extraction 138.6 kg, be cooled to 50 DEG C stand-by.
(2), the synthesis of emulsion splitter:
By front step silicone resin graft resin, hydro-oxidation sodium 15 kg, be warmed up to 120 DEG C-130 DEG C, more logical oxyethane 180 kg, propylene oxide 315 kg, reaction 3.5h, is cooled to 20 DEG C of blowings.
Corresponding chemical formula is:
Wherein R is C
8h
17-, Ph is phenyl, and Y is modified phenolic resins, the polyether type organic silicone resin in Xc-silicone resin, [X
c]-[Y] be silicone resin graft resin, Po is oxyethane, and PE is propylene oxide, A, B for link number, A is 18, B is 31, and Platinic chloride and sodium hydroxide are catalyzer.
Embodiment 3:
(1), the synthesis of silicone resin graft resin:
By silicone resin 50 kg of amino-functional, heptyl phenol 150 kg, formaldehyde 100 kg, Platinic chloride 0.08 kg, add in reactor, intensification degree 80-90 DEG C, reaction 2.5h, be cooled to 40 DEG C stand-by.
(2), the synthesis of emulsion splitter:
By front step silicone resin graft resin, hydro-oxidation potassium 12 kg, be warmed up to 120 DEG C-130 DEG C, more logical oxyethane 200 kg, propylene oxide 300 kg, reaction 5h, is cooled to 42 DEG C of blowings.
Corresponding chemical formula is:
Wherein R is C
7h
15-, Ph is phenyl, and Y is modified phenolic resins, [X
c]-[Y] be silicone resin graft resin, Po is oxyethane, and PE is propylene oxide, A, B for link number, A is 20, B is 30, and silicone resin Xc is the silicone resin of amino-functional, and structural formula is
Link number m, n be greater than 0 integer, Platinic chloride and potassium hydroxide are catalyzer.
Embodiment 4:
(1), the synthesis of silicone resin graft resin:
By hydrogeneous silicone resin 50 kg, base phenol 100 kg, formaldehyde 90-110 kg, Platinic chloride 0.08 kg, add in reactor, intensification degree 80-90 DEG C, reaction 2.5h, lowers the temperature stand-by.
(2), the synthesis of emulsion splitter:
By front step silicone resin graft resin, hydro-oxidation potassium 12 kg, be warmed up to 120 DEG C-130 DEG C, more logical oxyethane 200 kg, propylene oxide 350 kg, reaction 4h, is cooled to 40 DEG C of blowings.
Corresponding chemical formula is:
Wherein R is C
6h
13-, Ph is phenyl, and Y is modified phenolic resins, [X
c]-[Y] be silicone resin graft resin, Po is oxyethane, and PE is propylene oxide, A, B for link number, A is 20, B is 35, and silicone resin Xc is hydrogeneous silicone resin, and structural formula is
Link number n be greater than 0 integer, Platinic chloride and potassium hydroxide are catalyzer.
Embodiment 5:
(1), the synthesis of silicone resin graft resin:
By the silicone resin of hydrogeneous silicone resin and amino-functional and polyether type organic silicone resin 100kg, certain herbaceous plants with big flowers base phenol and base phenol 150 kg, formaldehyde (mass percentage concentration is 37%) 300 kg, catalyzer 1 Platinic chloride 1 kg, add in reactor, intensification degree 80-90 DEG C, reaction 3.5h, vacuum hydro-extraction 189kg, be cooled to 55 DEG C stand-by.
(2), the synthesis of emulsion splitter:
By front step silicone resin graft resin, add catalyzer 2 sodium ethylate 50 kg, be warmed up to 120 DEG C-130 DEG C, more logical oxyethane 200 kg, propylene oxide 450 kg, reaction 6h, is cooled to 60 DEG C of blowings.
Its corresponding chemical formula is:
Wherein R is alkyl, and Ph is phenyl, and Y is modified phenolic resins, Xc-silicone resin, [X
c]-[Y] be silicone resin graft resin, Po is oxyethane, and PE is propylene oxide, A, B for link number, A is 20, B is 45, and Platinic chloride and sodium ethylate are catalyzer.
Claims (6)
1. a silicone resin grafting crude oil demulsifier, is characterized in that: be made up of the raw material of following parts by weight:
Silicone resin 5-10 part
Alkylphenol 10-15 part
Oxyethane 15-20 part
Propylene oxide 30-45 part
Highly basic 1-5 part
Platinic chloride 0.05-0.1 part
Formaldehyde 9-11 part or
The formalin of equal quality,
The preparation method of described silicone resin grafting crude oil demulsifier, is characterized in that: comprise the following steps:
(1) synthesis of silicone resin graft resin: by silicone resin, alkylphenol, formaldehyde or formalin and Platinic chloride, add in reactor, is warming up to 80-90 DEG C and carries out building-up reactions, be then cooled to less than 60 DEG C;
(2) synthesis of emulsion splitter: step (1) gained reactant is added alkali catalyst, passes into oxyethane and propylene oxide, intensification 120-130 DEG C is carried out building-up reactions, blowing of then lowering the temperature.
2. silicone resin grafting crude oil demulsifier according to claim 1, it is characterized in that: silicone resin be phenyl official can silicone resin, polyether type organic silicone resin, the silicone resin of amino-functional, at least one of hydrogeneous silicone resin, alkylphenol be base phenol, heptyl phenol, octyl phenol, nonyl phenol, certain herbaceous plants with big flowers base phenol one or more.
3. silicone resin grafting crude oil demulsifier according to claim 1 and 2, is characterized in that: the mass percentage concentration of formalin is 37%, and addition is 25-30 part.
4. the preparation method of silicone resin grafting crude oil demulsifier according to claim 1, is characterized in that: comprise described step.
5. the preparation method of silicone resin grafting crude oil demulsifier according to claim 4, is characterized in that: add formalin in step (1), carry out processed after building-up reactions.
6. the preparation method of silicone resin grafting crude oil demulsifier according to claim 4, is characterized in that: in step (2), highly basic is potassium hydroxide.
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| CN201210508023.4A CN102942956B (en) | 2012-12-03 | 2012-12-03 | Organic silicon resin grafted crude oil demulsification agent and preparation method thereof |
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| CN104946298A (en) * | 2015-07-07 | 2015-09-30 | 万达集团股份有限公司 | Crude oil demulsifier and production technology thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0141585A2 (en) * | 1983-10-21 | 1985-05-15 | The British Petroleum Company p.l.c. | Demulsifying process |
| CN102432888A (en) * | 2011-08-15 | 2012-05-02 | 陕西科技大学 | Comb-type polysiloxane crude oil demulsifier and preparation method thereof |
-
2012
- 2012-12-03 CN CN201210508023.4A patent/CN102942956B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0141585A2 (en) * | 1983-10-21 | 1985-05-15 | The British Petroleum Company p.l.c. | Demulsifying process |
| CN102432888A (en) * | 2011-08-15 | 2012-05-02 | 陕西科技大学 | Comb-type polysiloxane crude oil demulsifier and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 原油破乳剂的合成方法;任朝华等;《精细石油化工进展》;20110331;第12卷(第3期);第45-48页 * |
| 高效稠油破乳剂LS938-2的研制与应用;孙吉佑等;《油田化学》;20041225;第21卷(第4期);第328-329页 * |
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