CN102942956A - 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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- CN102942956A CN102942956A CN2012105080234A CN201210508023A CN102942956A CN 102942956 A CN102942956 A CN 102942956A CN 2012105080234 A CN2012105080234 A CN 2012105080234A CN 201210508023 A CN201210508023 A CN 201210508023A CN 102942956 A CN102942956 A CN 102942956A
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- silicone resin
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- demulsification agent
- phenol
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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 the extraction process, and dehydration is one of important step in the petroleum production processes process.At present, the most frequently used reason breaking method of petroleum industry is to add emulsion splitter in crude oil, and the crude oil in China component is comparatively complicated, different geographical, different blocks, even there is not different difference in same oil well oil yet, and emulsion splitter has stronger specific aim, and this has strengthened 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, stability also worse and worse, this type of crude oil demulsification difficulty is increasing, the breakdown of emulsion temperature constantly raises, the scope of application is more and more narrow, can not meeting the market requirement.
(3) summary of the invention
The present invention adopts modern biofermentation technique, and a kind of high-low temperature resistant, applied widely, effective silicone resin grafting crude oil demulsifier and preparation method thereof are provided.
The present invention is achieved through the following technical solutions:
A kind of silicone resin grafting crude oil demulsifier, its special character is: the raw material by following parts by weight is made:
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.
Its corresponding chemical reaction is:
Wherein R is alkyl, and Ph is phenyl, and Y is modified phenolic resins, and Xc is silicone resin, [X
C]-[Y] be the silicone resin graft resin, Po is oxyethane, PE is propylene oxide, A, B are the integer in the 15-20 for link number, A, B is the integer in the 30-45, Platinic chloride and highly basic are catalyzer.
Silicone resin grafting crude oil demulsifier of the present invention, silicone resin be the phenyl official can silicone resin, polyether type organic silicone resin, the silicone resin of amino-functional, hydrogeneous silicone resin at least a, alkylphenol for basic phenol, heptyl phenol, octyl phenol, nonyl phenol, the basic phenol of certain herbaceous plants with big flowers one or more.
Silicone resin grafting crude oil demulsifier of the present invention, preferred formalin contains formaldehyde 9-11 part in raw material formaldehyde and the formalin in the formalin, and preferred, 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: may further comprise the steps: (1) silicone resin graft resin synthetic: with silicone resin, alkylphenol, formaldehyde or formalin and catalyzer Platinic chloride, add in the reactor, be warming up to 80-90 ℃ and carry out building-up reactions, then be cooled to below 60 ℃;
(2) emulsion splitter is synthetic: step (1) gained reactant is added alkali catalyst, pass into oxyethane and propylene oxide, intensification 120-130 ℃ is carried out building-up reactions, the blowing of then lowering the temperature.
Add formalin among the preparation method of silicone resin grafting crude oil demulsifier of the present invention, step (1), carry out processed after the building-up reactions.
Highly basic is potassium hydroxide among the preparation method of silicone resin grafting crude oil demulsifier of the present invention, step (2).
Technical scheme of the present invention, its major advantage is as follows:
(1) high temperature resistant, be conducive to emulsion splitter and be higher than 150 ℃ of stability under the high temperature;
(2) viscosity is low, is about 0.606mpas and mixing soon, has reduced 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, mix 5min and get final product layering.
(4) embodiment
Embodiment 1:
(1), the silicone resin grafting is synthetic:
With the phenyl official can silicone resin 60kg, nonyl phenol 130 kg, formaldehyde (mass percentage concentration is 37%) 250 kg, Platinic chloride 0.5 kg, add in the reactor, be warmed up to 80 ℃, keep 80-90 ℃ of temperature, reaction 3h, vacuum hydro-extraction 157.5 kg, be cooled to 60 ℃ stand-by.
(2), emulsion splitter is synthetic:
With front step silicone resin graft resin, hydro-oxidation potassium 10 kg, be warmed up to 120 ℃-130 ℃, pass into again 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, Y is modified phenolic resins, [X
C]-[Y] be the silicone resin graft resin, Po is oxyethane, PE is propylene oxide, A, B for the link number, A is 15, B is 40, silicone resin Xc be the phenyl official can silicone resin, structural formula is
Link number m, n are the integer greater than 0, and Platinic chloride and potassium hydroxide are catalyzer.
Embodiment 2:
(1), silicone resin grafting tree is synthetic:
With 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 the reactor, are warmed up to 80 ℃, continue temperature 80-90 ℃, the reaction 4h, vacuum hydro-extraction 138.6 kg, be cooled to 50 ℃ stand-by.
(2), emulsion splitter is synthetic:
With front step silicone resin graft resin, hydro-oxidation sodium 15 kg, be warmed up to 120 ℃-130 ℃, more logical oxyethane 180 kg, propylene oxide 315 kg, reaction 3.5h is cooled to 20 ℃ of blowings.
Corresponding chemical formula is:
Wherein R is C
8H
17-, Ph is phenyl, Y is modified phenolic resins, the polyether type organic silicone resin in the Xc-silicone resin, [X
C]-[Y] be the silicone resin graft resin, Po is oxyethane, PE is propylene oxide, A, B for the link number, A is 18, B is 31, Platinic chloride and sodium hydroxide are catalyzer.
Embodiment 3:
(1), the silicone resin graft resin is synthetic:
With silicone resin 50 kg, heptyl phenol 150 kg, formaldehyde 100 kg, Platinic chloride 0.08 kg of amino-functional, add in the reactor, 80-90 ℃ of intensification degree, reaction 2.5h, be cooled to 40 ℃ stand-by.
(2), emulsion splitter is synthetic:
With front step silicone resin graft resin, hydro-oxidation potassium 12 kg, be warmed up to 120 ℃-130 ℃, more logical oxyethane 200 kg, propylene oxide 300 kg, reaction 5h is cooled to 42 ℃ of blowings.
Corresponding chemical formula is:
Wherein R is C
7H
15-, Ph is phenyl, Y is modified phenolic resins, [X
C]-[Y] be the silicone resin graft resin, Po is oxyethane, PE is propylene oxide, A, B for the link number, A is 20, B is 30, silicone resin Xc is the silicone resin of amino-functional, structural formula is
Link number m, n are the integer greater than 0, and Platinic chloride and potassium hydroxide are catalyzer.
Embodiment 4:
(1), the silicone resin graft resin is synthetic:
With hydrogeneous silicone resin 50 kg, basic phenol 100 kg, formaldehyde 90-110 kg, Platinic chloride 0.08 kg, add in the reactor, 80-90 ℃ of intensification degree, reaction 2.5h lowers the temperature stand-by.
(2), emulsion splitter is synthetic:
With front step silicone resin graft resin, hydro-oxidation potassium 12 kg, be warmed up to 120 ℃-130 ℃, more logical oxyethane 200 kg, propylene oxide 350 kg, reaction 4h is cooled to 40 ℃ of blowings.
Corresponding chemical formula is:
Wherein R is C
6H
13-, Ph is phenyl, Y is modified phenolic resins, [X
C]-[Y] be the silicone resin graft resin, Po is oxyethane, PE is propylene oxide, A, B for the link number, A is 20, B is 35, silicone resin Xc is hydrogeneous silicone resin, structural formula is
Link number n is the integer greater than 0, and Platinic chloride and potassium hydroxide are catalyzer.
Embodiment 5:
(1), the silicone resin graft resin is synthetic:
Silicone resin and polyether type organic silicone resin 100kg, the certain herbaceous plants with big flowers base phenol of hydrogeneous silicone resin and amino-functional are reached basic phenol 150 kg, formaldehyde (mass percentage concentration is 37%) 300 kg, catalyzer 1 Platinic chloride 1 kg, add in the reactor, 80-90 ℃ of intensification degree, reaction 3.5h, vacuum hydro-extraction 189kg, be cooled to 55 ℃ stand-by.
(2), emulsion splitter is synthetic:
With front step silicone resin graft resin, add catalyzer 2 sodium ethylates 50 kg, be warmed up to 120 ℃-130 ℃, logical oxyethane 200 kg, propylene oxide 450 kg react 6h again, are cooled to 60 ℃ 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 the silicone resin graft resin, Po is oxyethane, PE is propylene oxide, A, B for the link number, A is 20, B is 45, Platinic chloride and sodium ethylate are catalyzer.
Claims (6)
1. silicone resin grafting crude oil demulsifier, it is characterized in that: the raw material by following parts by weight is made:
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.
2. silicone resin grafting crude oil demulsifier according to claim 1, it is characterized in that: silicone resin be the phenyl official can silicone resin, polyether type organic silicone resin, the silicone resin of amino-functional, hydrogeneous silicone resin at least a, alkylphenol for basic phenol, heptyl phenol, octyl phenol, nonyl phenol, the basic phenol of certain herbaceous plants with big flowers one or more.
3. silicone resin grafting crude oil demulsifier according to claim 1 and 2, it is characterized in that: the mass percentage concentration of formalin is 37%, addition is 25-30 part.
4. the preparation method of silicone resin grafting crude oil demulsifier according to claim 1 is characterized in that: may further comprise the steps:
(1) the silicone resin graft resin is synthetic: with silicone resin, alkylphenol, formaldehyde or formalin and Platinic chloride add in the reactor, are warming up to 80-90 ℃ and carry out building-up reactions, then are cooled to below 60 ℃;
(2) emulsion splitter is synthetic: step (1) gained reactant is added alkali catalyst, pass into oxyethane and propylene oxide, intensification 120-130 ℃ is carried out building-up reactions, the blowing of then lowering the temperature.
5. the preparation method of silicone resin grafting crude oil demulsifier according to claim 4 is characterized in that: add formalin in the step (1), carry out processed after the building-up reactions.
6. the preparation method of silicone resin grafting crude oil demulsifier according to claim 4 is characterized in that: highly basic is potassium hydroxide in the step (2).
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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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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
|---|
| 任朝华等: "原油破乳剂的合成方法", 《精细石油化工进展》 * |
| 孙吉佑等: "高效稠油破乳剂LS938-2的研制与应用", 《油田化学》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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