CN102504246B - Method for preparing polyepichlorohydrin-diethanol amine anti-collapse inhibitor in laboratory - Google Patents
Method for preparing polyepichlorohydrin-diethanol amine anti-collapse inhibitor in laboratory Download PDFInfo
- Publication number
- CN102504246B CN102504246B CN201110340245.5A CN201110340245A CN102504246B CN 102504246 B CN102504246 B CN 102504246B CN 201110340245 A CN201110340245 A CN 201110340245A CN 102504246 B CN102504246 B CN 102504246B
- Authority
- CN
- China
- Prior art keywords
- water
- parts
- diethanolamine
- necked flask
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Epoxy Resins (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for preparing a polyepichlorohydrin-diethanol amine anti-collapse inhibitor in a laboratory. The method comprises the following main steps of: adding 10-30 parts of diethanol amine into 10-20 parts of water in volume; after uniformly mixing, slowly dropping 10-30 parts of epoxy chloropropane while stirring; and then stirring at 30-60 DEG C and reacting at constant temperature for 2-5 h so as to obtain colourless or faint yellow sticky liquid, namely an anti-collapse inhibitor product. The inhibitor has high positive charge density, contains a lot of hydroxyls and is capable of entering intercalated clay or being adsorbed on the surface of the intercalated clay; electric double-layer thicknesses of clay particles can be compressed through electrical neutralization action, so that clay hydration expansion can be effectively inhibited; and the inhibitor has a steady property and good compatibility with the common drilling fluid additive and can be widely applied to the drilling fluid systems, such as polymers, cationic sol, solid-free phases and the like.
Description
Technical field
The laboratory preparation method who the present invention relates to a kind of Hydrin-diethanolamine anti-collapse inhibitor, this inhibitor is mainly used as water-base drilling fluid treatment agent, belongs to petroleum drilling fluid technical field.
Background technology
Hole collapse is a great problem of puzzlement drilling engineering.Anti-collapse inhibitor is to improve property of drilling fluid, improves the core of wellbore stability technology.At present, conventional drilling fluid mainly contains with mud shale anti-collapse inhibitor: pitch class, polymer class and inorganic salts etc.These anti-collapse inhibitors all come with some shortcomings separately: as pitch class is unfavorable for environment protection; Silicate can make system rheological be difficult to control; Glucosides class, polyethylene glycols, can not solve the drilling problem of active mud shale; The amido inhibitor of exploitation in recent years, because complicated process of preparation, cost are too high, domesticly also not yet forms ripe production technique, lacks the preparation method that production technique is simple and direct, is difficult to meet the stable demand of mud shale drilling shaft lining.
Summary of the invention
The object of the invention is to provide a kind of laboratory preparation method of Hydrin-diethanolamine anti-collapse inhibitor, select suitable group to organically combine from the angle of molecular designing, thereby develop the water-base drilling fluid inhibitor that is suitable for application, and progressively foundation trips out corresponding simple and direct preparation method, meets the stable demand of mud shale drilling shaft lining.
The present invention adopts following technical scheme, and a kind of laboratory preparation method of Hydrin-diethanolamine anti-collapse inhibitor comprises the steps:
The preparation of the first step feed chemicals
According to volume parts, every part is no less than 1mL, prepares following material:
10～20 parts, water;
10～30 parts of epoxy chloropropane;
10～30 parts of diethanolamine;
The water-bath of second step low temperature
Select in the there-necked flask of 150mL, each mouthful of there-necked flask is used separately as puts thermometer, agitator and interpolation feed chemicals, gets 10～20 parts of water and joins in there-necked flask, and there-necked flask is placed in ice-water bath, and its temperature is controlled at below 25 DEG C;
The 3rd step adds diethanolamine
Completing in the there-necked flask of previous step requirement, add the diethanolamine of 10～30 parts, stir 10 minutes, until diethanolamine mixes completely with water, keep during this time low temperature water-bath, its temperature is controlled at below 25 DEG C;
The 4th step drips epoxy chloropropane
10～30 parts of epoxy chloropropane are added to dropping funnel, the thermometer changing-over that former flask mouth is placed is condenser, open the water coolant of reflux exchanger, under stirring state, with 30 minutes, epoxy chloropropane is added drop-wise in flask, in whole dropping process, keep low temperature water-bath, the temperature in there-necked flask is controlled at below 25 DEG C;
The 5th step continues to stir
After dropwising, maintain the interior temperature of there-necked flask below 25 DEG C, then continue to stir 30 minutes;
The 6th step heats up and keeps isothermal reaction, obtains product
Bath temperature is increased to a certain temperature between 30 DEG C～60 DEG C, keeps isothermal reaction 2～5 hours, obtain Hydrin-diethanolamine anti-collapse inhibitor product.
This anti-collapse inhibitor product appearance is faint yellow or colourless viscous liquid, after tested, the feed stock conversion > 90% of above-mentioned reaction, solid load is: 65% to 80%, positive charge density is at 5～6mmolg-1.This agent positive charge density is high, with great amount of hydroxy group, can enter between clay seam or be adsorbed on its surface, by charge neutrality effect compression clay particle electrostatic double layer thickness, thereby effectively suppress hydration and expansion of clay.
The laboratory preparation method of above-mentioned Hydrin-diethanolamine anti-collapse inhibitor, its chemical equation is as follows:
The product that the inventive method is obtained and polymeric alcohol and KCl rejection compare:
Adopt and measure the roll back method of yield of mud shale landwaste heat its inhibition is evaluated.Get North China Oilfield man 11 well landwaste and cross 6～10 mesh sieves, dry to constant weight, take four parts of each 50g of landwaste, add respectively in clear water, 2% product solution of the present invention, 2% polymeric alcohol solution and 2%KCl solution, under 80 DEG C of conditions, heat is rolled 16 hours, cooling after, after rinsing well with 40 eye mesh screens, put into baking oven, dry to constant weight at 105 DEG C, weigh, calculate recovery rate.
Evaluation result is as shown in following table 1 " product of the present invention and polymeric alcohol, KCl inhibition comparative result ": the in the situation that of identical dosage, the prepared product rejection of the present invention is obviously better than polymeric alcohol and KCl, and the landwaste rolling rate of recovery improves 50.95% compared with clear water.
Table 1. product of the present invention and polymeric alcohol, KCl inhibition comparative result
| Solution title | The rolling rate of recovery (%) |
| Clear water | 22.75 |
| 2% product solution of the present invention | 73.70 |
| 2% polymeric alcohol solution | 45.75 |
| 2%KCl solution | 52.50 |
By product application of the present invention in polymkeric substance, positive colloid and evaluate without the effect in the drilling fluid systems such as solid phase respectively to the product of the present invention that adds 2% in following three kinds of conventional drilling liquid system, investigate its impact on drilling fluid properties, in table 2 " effect before and after the dosing of product of the present invention in polymkeric substance, positive colloid and clay-free drilling fluid system ".
1, polymer drilling fluid system: 5% wilkinite+0.3%KPAM+1.5%SMP-2+1.5%FT-103;
2, Mmh Drilling Fluid System: 5% wilkinite+0.5% positive colloid+1%L-CMC+0.5%NPAN;
3, clay-free drilling fluid system: clear water+0.2% sodium carbonate+0.4%XP+0.2%L-XC+1.5% starch+1.5% albino bitumen+organic salt;
Effect before and after the dosing of table 2. product of the present invention in polymkeric substance, positive colloid and clay-free drilling fluid system
In above-mentioned literary composition, relate to code name and nomenclature
KCl: Repone K; KPAM: polyacrylic acid potassium; SMP-2: sulfonated phenol formaldehyde resin; FT-103: anti-collapse and anti-falling filtration agent; L-CMC: low sticky carboxymethyl cellulose; XP: biological polymer; NPAN: hydrolyzed polyacrylonitrile ammonium salt; L-XC: low sticky xanthan gum; AV: apparent viscosity, mPas; PV: plastic viscosity, mPas; Gels: just/10-minute gel strength, Pa; FL:API filter loss, mL.
Experimental data in table 2 shows: product of the present invention is all little on three kinds of drilling fluid rheologies and API filtration impact, the rolling rate of recovery but obviously improves, especially positive colloid and polymeric system inhibition are had to larger improvement, this Hydrin-diethanolamine anti-collapse inhibitor and common drilling fluid treatment agent have good compatibleness.
Embodiment
Below in conjunction with embodiment, the laboratory preparation method of Hydrin-diethanolamine anti-collapse inhibitor of the present invention is further described.
Embodiment mono-:
The laboratory preparation of Hydrin-diethanolamine anti-collapse inhibitor
The preparation of the first step feed chemicals
According to volume parts, every part is no less than 1mL, prepares as follows:
10 parts, water;
20 parts of epoxy chloropropane;
20 parts of diethanolamine;
The water-bath of second step low temperature
Select in the there-necked flask of 150mL, each mouthful of there-necked flask is used separately as puts thermometer, agitator and interpolation feed chemicals, gets 10mL water and joins in there-necked flask, and there-necked flask is placed in ice-water bath, and its temperature is controlled at below 25 DEG C;
The 3rd step adds diethanolamine
Completing in the there-necked flask of previous step requirement, add the diethanolamine of 20mL, stir 10 minutes, until diethanolamine mixes completely with water, keep during this time low temperature water-bath, its temperature is controlled at below 25 DEG C;
The 4th step drips epoxy chloropropane
15.6mL epoxy chloropropane is added to dropping funnel, the thermometer changing-over that former flask mouth is placed is condenser, open the water coolant of reflux exchanger, under stirring state, with 30 minutes, epoxy chloropropane is added drop-wise in flask, in whole dropping process, keep low temperature water-bath, the temperature in there-necked flask is controlled at below 25 DEG C;
The 5th step continues to stir
After dropwising, maintain the interior temperature of there-necked flask below 25 DEG C, then continue to stir 30 minutes;
The 6th step heats up and keeps isothermal reaction, obtains product
Bath temperature is increased to 40 DEG C, keeps isothermal reaction 4 hours, obtain Hydrin-diethanolamine anti-collapse inhibitor product.
Embodiment bis-: the laboratory preparation of Hydrin-diethanolamine anti-collapse inhibitor
The preparation of the first step feed chemicals
According to volume parts, every part is no less than 1mL, prepares as follows:
20 parts, water;
30 parts of epoxy chloropropane;
30 parts of diethanolamine;
The water-bath of second step low temperature
Select in the there-necked flask of 150mL, each mouthful of there-necked flask is used separately as puts thermometer, agitator and interpolation feed chemicals, gets 20mL water and joins in there-necked flask, and there-necked flask is placed in ice-water bath, and its temperature is controlled at below 25 DEG C;
The 3rd step adds diethanolamine
Completing in the there-necked flask of previous step requirement, add the diethanolamine of 30mL, stir 10 minutes, until diethanolamine mixes completely with water, keep during this time low temperature water-bath, its temperature is controlled at below 25 DEG C;
The 4th step drips epoxy chloropropane
26mL epoxy chloropropane is added to dropping funnel, the thermometer changing-over that former flask mouth is placed is condenser, open the water coolant of reflux exchanger, under stirring state, with 30 minutes, epoxy chloropropane is added drop-wise in flask, in whole dropping process, keep low temperature water-bath, the temperature in there-necked flask is controlled at below 25 DEG C;
The 5th step continues to stir
After dropwising, maintain the interior temperature of there-necked flask below 25 DEG C, then continue to stir 30 minutes;
The 6th step heats up and keeps isothermal reaction, obtains product
Bath temperature is increased to 60 DEG C, keeps isothermal reaction 3.5 hours, obtain Hydrin-diethanolamine anti-collapse inhibitor product.
Embodiment tri-: the laboratory preparation of Hydrin-diethanolamine anti-collapse inhibitor
The preparation of the first step feed chemicals
According to volume parts, every part is no less than 1mL, prepares as follows:
10 parts, water;
20 parts of epoxy chloropropane;
20 parts of diethanolamine;
The water-bath of second step low temperature
Select in the there-necked flask of 150mL, each mouthful of there-necked flask is used separately as puts thermometer, agitator and interpolation feed chemicals, gets 10mL water and joins in there-necked flask, and there-necked flask is placed in ice-water bath, and its temperature is controlled at below 25 DEG C;
The 3rd step adds diethanolamine
Completing in the there-necked flask of previous step requirement, add the diethanolamine of 20mL, stir 10 minutes, until diethanolamine mixes completely with water, keep during this time low temperature water-bath, its temperature is controlled at below 25 DEG C;
The 4th step drips epoxy chloropropane
20mL epoxy chloropropane is added to dropping funnel, the thermometer changing-over that former flask mouth is placed is condenser, open the water coolant of reflux exchanger, under stirring state, with 30 minutes, epoxy chloropropane is added drop-wise in flask, in whole dropping process, keep low temperature water-bath, the temperature in there-necked flask is controlled at below 25 DEG C;
The 5th step continues to stir
After dropwising, maintain the interior temperature of there-necked flask below 25 DEG C, then continue to stir 30 minutes;
The 6th step heats up and keeps isothermal reaction, obtains product
Bath temperature is increased to 30 DEG C, keeps isothermal reaction 5 hours, obtain Hydrin-diethanolamine anti-collapse inhibitor product.
According to the laboratory preparation method of Hydrin-diethanolamine anti-collapse inhibitor of the present invention, under the different components limiting and condition variation, all can generate Hydrin-diethanolamine.
Utilize method of the present invention to prepare Hydrin-diethanolamine anti-collapse inhibitor and correlated process process control method; and derive from creation thought essence of the present invention, just in equipment and envrionment conditions, improved method all belongs to the scope of protection of the invention.
Claims (1)
1. a laboratory preparation method for Hydrin-diethanolamine anti-collapse inhibitor, comprises the steps:
The preparation of the first step feed chemicals
According to volume parts, every part is no less than 1mL, prepares following material:
10～20 parts, water;
10～30 parts of epoxy chloropropane;
10～30 parts of diethanolamine;
The water-bath of second step low temperature
Select in the there-necked flask of 150mL, each mouthful of there-necked flask is used separately as puts thermometer, agitator and interpolation feed chemicals, gets 10～20 parts of water and joins in there-necked flask, and there-necked flask is placed in ice-water bath, and its temperature is controlled at below 25 DEG C;
The 3rd step adds diethanolamine
Completing in the there-necked flask of previous step requirement, add the diethanolamine of 10～30 parts, stir 10 minutes, until diethanolamine mixes completely with water, keep during this time low temperature water-bath, its temperature is controlled at below 25 DEG C;
The 4th step drips epoxy chloropropane
10～30 parts of epoxy chloropropane are added to dropping funnel, the thermometer changing-over that former flask mouth is placed is condenser, open the water coolant of reflux exchanger, under stirring state, with 30 minutes, epoxy chloropropane is added drop-wise in flask, in whole dropping process, keep low temperature water-bath, the temperature in there-necked flask is controlled at below 25 DEG C;
The 5th step continues to stir
After dropwising, maintain the interior temperature of there-necked flask below 25 DEG C, then continue to stir 30 minutes;
The 6th step heats up and keeps isothermal reaction, obtains product
Bath temperature is increased to a certain temperature between 30 DEG C～60 DEG C, keeps isothermal reaction 2～5 hours, obtain Hydrin-diethanolamine anti-collapse inhibitor product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110340245.5A CN102504246B (en) | 2011-11-02 | 2011-11-02 | Method for preparing polyepichlorohydrin-diethanol amine anti-collapse inhibitor in laboratory |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110340245.5A CN102504246B (en) | 2011-11-02 | 2011-11-02 | Method for preparing polyepichlorohydrin-diethanol amine anti-collapse inhibitor in laboratory |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102504246A CN102504246A (en) | 2012-06-20 |
| CN102504246B true CN102504246B (en) | 2014-06-18 |
Family
ID=46216384
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110340245.5A Expired - Fee Related CN102504246B (en) | 2011-11-02 | 2011-11-02 | Method for preparing polyepichlorohydrin-diethanol amine anti-collapse inhibitor in laboratory |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102504246B (en) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103087689B (en) * | 2013-02-05 | 2015-06-10 | 四川仁智油田技术服务股份有限公司 | High temperature resistance and viscosity reduction agent for water-based drilling fluid |
| CN103571442B (en) * | 2013-11-18 | 2016-08-31 | 淄博职业学院 | A kind of preparation method and application of the clay inhibitor of melamine-derived |
| CN104529222B (en) * | 2014-12-22 | 2016-09-14 | 西南科技大学 | A kind of retardation setting type cement grinding aid and preparation method thereof |
| CN105802592A (en) * | 2016-04-07 | 2016-07-27 | 西南石油大学 | Shale inhibitor as well as preparation method and application thereof |
| CN109694697A (en) * | 2017-10-23 | 2019-04-30 | 中石化石油工程技术服务有限公司 | A kind of drilling fluid polyamine shale inhibitor and preparation method thereof and drilling fluid |
| CN108070365B (en) * | 2017-12-14 | 2020-06-05 | 贵州省地质矿产勘查开发局一一五地质大队 | Water-based drilling fluid suitable for coal-series stratum drilling and preparation method thereof |
| CN113445747A (en) * | 2021-06-28 | 2021-09-28 | 福建伯裕堡建筑科技发展有限公司 | Rigid composite waterproof structure containing FJT waterproof compacting agent and construction method thereof |
| CN116426256B (en) * | 2021-12-30 | 2024-08-16 | 中国石油化工股份有限公司 | Antiwear drag reduction treating agent, preparation method, lubricant composition and application |
| CN117363333A (en) * | 2022-06-29 | 2024-01-09 | 中国石油天然气集团有限公司 | Temperature-resistant and salt-resistant organic metal crosslinking agent, and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101311240A (en) * | 2007-05-24 | 2008-11-26 | 新疆石油管理局钻井工艺研究院 | Glucoheptonate restraining agent for drilling fluid and method for preparing same |
-
2011
- 2011-11-02 CN CN201110340245.5A patent/CN102504246B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101311240A (en) * | 2007-05-24 | 2008-11-26 | 新疆石油管理局钻井工艺研究院 | Glucoheptonate restraining agent for drilling fluid and method for preparing same |
Non-Patent Citations (2)
| Title |
|---|
| 李柏林等.环氧氯丙烷-二乙醇胺共聚物合成研究.《化学与生物工程》.2009,第26卷(第11期),30-32. |
| 环氧氯丙烷-二乙醇胺共聚物合成研究;李柏林等;《化学与生物工程》;20091130;第26卷(第11期);30-32 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102504246A (en) | 2012-06-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102504246B (en) | Method for preparing polyepichlorohydrin-diethanol amine anti-collapse inhibitor in laboratory | |
| CN100513508C (en) | Oil-soluble cationic broad-spectrum temporary plugging agent for drilling fluid | |
| CN102863947A (en) | Strong-inhibition strong-blocking drilling fluid | |
| CN102352232B (en) | Temperature-resistant and salt-resistant polymer clean fracturing fluid thickening agent and preparation method thereof | |
| CN102070909A (en) | Cation modified asphalt and preparation method thereof | |
| CN106318347A (en) | Silicate-aluminate anti-sloughing drilling fluid | |
| CN104558217B (en) | cross-linked starch for drilling fluid and preparation method thereof | |
| CN101624516A (en) | Fluid loss additive of oil-base drilling fluid and preparation method thereof | |
| CN102373037B (en) | Novel biological blockage removing solution for well completion, and production method thereof | |
| CN103497755A (en) | Method for manufacturing fracturing fluid | |
| CN109233762A (en) | A kind of drilling fluid, preparation method and application | |
| CN102863584A (en) | Preparation method for macromolecule emulsion coating agent for drilling fluid | |
| CN104962252A (en) | Organic salt polyamine drilling fluid and preparation method thereof | |
| CN107312507B (en) | Clay stabilizer and application thereof | |
| CN107488247B (en) | A kind of preparation method of polymer for drilling fluid shale control agent | |
| ITUB20150203A1 (en) | INHIBITORS OF SHISTS | |
| CN103483500A (en) | High-temperature resistant and strong water-absorbing fluid loss additive and application thereof | |
| CN103952128B (en) | It is applicable to the Weak Gels Solid Free water-base drilling fluid of extended reach well, horizontal well | |
| CN102796503B (en) | Intercalation polymer gel diverting agent | |
| CN105385425A (en) | Palm oil base well drilling fluid and preparation method thereof | |
| CN112111039B (en) | Dispersing agent, preparation method and application thereof | |
| CN104531102A (en) | Natural polymer filtrate loss reducer used for drilling fluid and preparation method and application thereof | |
| CN204079497U (en) | The dry machine of organic bentonite production rake | |
| CN105601803B (en) | A kind of synthetic method of slippery water drag reducer | |
| CN103571442A (en) | Preparation method and application of clay inhibitor derived from melamine |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140618 Termination date: 20171102 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |