CN107345129A - A kind of Waterproof lock agent and preparation method thereof - Google Patents
A kind of Waterproof lock agent and preparation method thereof Download PDFInfo
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- CN107345129A CN107345129A CN201710510691.3A CN201710510691A CN107345129A CN 107345129 A CN107345129 A CN 107345129A CN 201710510691 A CN201710510691 A CN 201710510691A CN 107345129 A CN107345129 A CN 107345129A
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- waterproof lock
- lock agent
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
Abstract
The present invention relates to a kind of Waterproof lock agent and preparation method thereof, belong to drilling fluid additive technical field.Acrylamide, distilled water, glycerin monostearate and cetyltriethylammonium bromide are put into mixer by the present invention to be stirred, and is collected stirring mixture, is obtained emulsion；Emulsion, hexamethylene, liquid polybutadiene, ammonium metavanadate and neodymia are put into reactor, protected using nitrogen, is preheated, adds ammonium persulfate, is stirred；After stirring terminates, heated up simultaneously stirring reaction, and γ aminopropyl triethoxysilanes are added after cooling, are stirred, are stood, are cooled to room temperature, collect reactant mixture；Reactant mixture is evaporated under reduced pressure, removal distilled water and hexamethylene, collects distillation residue, filtering, collect filtered fluid, filtered fluid and Sitosterolum are stirred, you can obtain Waterproof lock agent.Waterproof lock agent prepared by the present invention effectively reduces the tension force and oil water interfacial tension of filtrate surface, improves oil, gas phase permeability.
Description
Technical field
The present invention relates to a kind of Waterproof lock agent and preparation method thereof, belong to drilling fluid additive technical field.
Background technology
Low hole, low permeability reservoirs typically have high argillaceous cement content, water saturation height, capillary pressure height, water
Quick property is strong and pore throat is tiny, poor permeability, it is complicated, oil gas flow resistance is big the features such as.Numerous studies show, Water-blocking damage
It is that the type reservoir is main, and the infringement type of most serious, loss ratio are generally 70%~90%.Drilling fluid is connect with reservoir
And ρ
Phase permeability reduces, and Waterproof lock agent is a kind of important additives used in drilling fluid system, by reducing drilling fluid filtrate table
Face tension force, prevent drilling fluid filtrate invaded formation from causing water to lock.Reduce water-blocking effect be the low hole of protection, low permeability reservoirs it is important
Measure.
Currently used Waterproof lock agent has：The surfactants such as OP-10, ABS and Tween, still, for low hole, hypotonic
The oil and gas reservoir of complex geologic conditions is waited thoroughly, and these Waterproof lock agent can not effectively reduce the surface tension and oil-water interfaces of filtrate
Power, to improve gas phase relative permeability.
It would therefore be highly desirable to a kind of tension force and oil-water interfaces ability that can effectively reduce filtrate surface is found, so as to improve oil, gas
The Waterproof lock agent of phase permeability.
The content of the invention
The technical problems to be solved by the invention：Filtrate surface can not be effectively reduced for Waterproof lock agent traditional at present
Tension force and oil water interfacial tension, cause the problem of oily, gas phase permeability is low, there is provided a kind of Waterproof lock agent and preparation method thereof.
In order to solve the above technical problems, the present invention is using technical scheme as described below：
A kind of Waterproof lock agent, it is characterised in that include the raw material of following parts by weight, 40~45 parts of hexamethylenes, 21~25 parts of liquid
Body polybutadiene, 20~28 parts of acrylamides, 15~20 parts of glycerin monostearates, 12~14 parts of distilled water, 10~15 parts of β-
Sitosterol, 4~6 parts of cetyltriethylammonium bromides, 3~5 parts of gamma-aminopropyl-triethoxy-silanes, 2~3 parts of ammonium persulfates,
0.4~0.6 part of ammonium metavanadate, 0.1~0.8 part of neodymia.
The mean molecule quantity of described liquid polybutadiene is 4000~10000.
The preparation method of Waterproof lock agent of the present invention comprises the following steps：
（1）Match in parts by weight, take raw material；
（2）Acrylamide, distilled water, glycerin monostearate and cetyltriethylammonium bromide are put into mixer and carried out
Stirring, stirring mixture is collected, obtains emulsion；
（3）Emulsion, hexamethylene, liquid polybutadiene, ammonium metavanadate and neodymia are put into reactor, protected using nitrogen
Shield, is preheated at 50~60 DEG C, adds ammonium persulfate, is stirred；
（4）After stirring terminate, 90~105 DEG C are warming up to, stirring reaction, gamma-aminopropyl-triethoxy-silane is added after cooling,
Stir, stand 6~9h, be cooled to room temperature, collect reactant mixture；
（5）Reactant mixture is evaporated under reduced pressure, removes distilled water and hexamethylene, collects distillation residue, and is filtered,
Filtered fluid is collected, filtered fluid and cupreol are stirred, collects stirring mixture, you can obtain Waterproof lock agent.
The step（4）In be cooled to temperature as 70~75 DEG C.
Compared with other method, advantageous effects are the present invention：
（1）The present invention is used as initiator, glycerin monostearate and cetyltriethylammonium bromide conduct by the use of ammonium persulfate
Emulsifying agent, by being stirred acquisition emulsifying agent with distilled water, hexamethylene is reused as solvent, in ammonium metavanadate and neodymia
Catalytic action under, acrylamide and liquid polybutadiene is carried out reactive polymeric, form high active surfactant, can be effective
Reduce the tension force and oil water interfacial tension of filtrate surface；
（2）The present invention uses cupreol to improve the efficiency of surfactant as surfactant adjuvant, further improve anti-
Water locks the efficiency of agent, while adds gamma-aminopropyl-triethoxy-silane improvement structural behaviour, increases the adhesive force in reservoir, more
Good reaches effect, and then improves the efficiency of Waterproof lock agent.
Embodiment
The Waterproof lock agent of the present invention, includes the raw material of following parts by weight, 40~45 parts of hexamethylenes, 21~25 parts of liquid gather
Butadiene, 20~28 parts of acrylamides, 15~20 parts of glycerin monostearates, 12~14 parts of distilled water, 10~15 parts of β-paddy steroid
Alcohol, 4~6 parts of cetyltriethylammonium bromides, 3~5 parts of gamma-aminopropyl-triethoxy-silanes, 2~3 parts of ammonium persulfates, 0.4
~0.6 part of ammonium metavanadate, 0.1~0.8 part of neodymia.
The mean molecule quantity of liquid polybutadiene in raw material is 4000~10000.
The preparation of Waterproof lock agent of the present invention comprises the following steps：
（1）Match in parts by weight, take raw material；
（2）Acrylamide, distilled water, glycerin monostearate and cetyltriethylammonium bromide are put into mixer, with
900r/min is stirred 20~30min, collects stirring mixture, obtains emulsion；
（3）Emulsion, hexamethylene, liquid polybutadiene, ammonium metavanadate and neodymia are put into reactor, protected using nitrogen
Shield, and 0.2~0.4MPa is boosted to, 10~15min of preheating is stirred with 200r/min at 50~60 DEG C, adds persulfuric acid
Ammonium, stir 30~35min；
（4）After stirring terminates, 90~105 DEG C are warming up to, 8~12h of stirring reaction, is cooled to 70~75 DEG C, adds γ-ammonia
Propyl-triethoxysilicane, stir, stand 6~9h, be cooled to room temperature, collect reactant mixture；
（5）Reactant mixture is put into distilling apparatus, is evaporated under reduced pressure, pressure is 0.02~0.04MPa, removes distilled water
And hexamethylene, distillation residue is collected, is stood overnight at 0 DEG C, and filtered, filtered fluid is collected, by filtered fluid and β-paddy
Sterol stirs, and collects stirring mixture, you can obtain Waterproof lock agent.
Example 1
The Waterproof lock agent of the present invention, includes the raw materials of following parts by weight, 45 parts of hexamethylenes, 25 parts of liquid polybutadienes, 28 parts
Acrylamide, 20 parts of glycerin monostearates, 14 parts of distilled water, 15 parts of cupreols, 6 parts of cetyltriethylammonium bromides, 5
Part gamma-aminopropyl-triethoxy-silane, 3 parts of ammonium persulfates, 0.6 part of ammonium metavanadate, 0.8 part of neodymia.
The mean molecule quantity of liquid polybutadiene in raw material is 10000.（Suzhou henry Shunda Chemical Industry Science Co., Ltd gives birth to
Production, model LPB-1）
The preparation of Waterproof lock agent of the present invention comprises the following steps：
（1）Match in parts by weight, take raw material；
（2）Acrylamide, distilled water, glycerin monostearate and cetyltriethylammonium bromide are put into mixer, with
900r/min is stirred 30min, collects stirring mixture, obtains emulsion；
（3）Emulsion, hexamethylene, liquid polybutadiene, ammonium metavanadate and neodymia are put into reactor, protected using nitrogen
Shield, and 0.4MPa is boosted to, preheating 15min is stirred with 200r/min at 60 DEG C, adds ammonium persulfate, stirs 35min；
（4）After stirring terminates, 105 DEG C are warming up to, stirring reaction 12h, is cooled to 75 DEG C, add the ethoxy of γ-aminopropyl three
Base silane, stir, stand 9h, be cooled to room temperature, collect reactant mixture；
（5）Reactant mixture is put into distilling apparatus, is evaporated under reduced pressure, pressure 0.04MPa, removes distilled water and hexamethylene
Alkane, distillation residue is collected, is stood overnight at 0 DEG C, and filtered, collected filtered fluid, filtered fluid and cupreol are stirred
Mix uniformly, collect stirring mixture, you can obtain Waterproof lock agent.
Example 2
The Waterproof lock agent of the present invention, includes the raw materials of following parts by weight, 40 parts of hexamethylenes, 21 parts of liquid polybutadienes, 20 parts
Acrylamide, 15 parts of glycerin monostearates, 12 parts of distilled water, 10 parts of cupreols, 4 parts of cetyltriethylammonium bromides, 3
Part gamma-aminopropyl-triethoxy-silane, 2 parts of ammonium persulfates, 0.4 part of ammonium metavanadate, 0.1 part of neodymia.
The mean molecule quantity of liquid polybutadiene in raw material is 4000.（The production of Shanghai Dong Hu Industrial Co., Ltd.s, type
Number it is Polyvest110）
The preparation of Waterproof lock agent of the present invention comprises the following steps：
（1）Match in parts by weight, take raw material；
（2）Acrylamide, distilled water, glycerin monostearate and cetyltriethylammonium bromide are put into mixer, with
900r/min is stirred 30min, collects stirring mixture, obtains emulsion；
（3）Emulsion, hexamethylene, liquid polybutadiene, ammonium metavanadate and neodymia are put into reactor, protected using nitrogen
Shield, and 0.4MPa is boosted to, preheating 15min is stirred with 200r/min at 60 DEG C, adds ammonium persulfate, stirs 35min；
（4）After stirring terminates, 105 DEG C are warming up to, stirring reaction 12h, is cooled to 75 DEG C, add the ethoxy of γ-aminopropyl three
Base silane, stir, stand 9h, be cooled to room temperature, collect reactant mixture；
（5）Reactant mixture is put into distilling apparatus, is evaporated under reduced pressure, pressure 0.04MPa, removes distilled water and hexamethylene
Alkane, distillation residue is collected, is stood overnight at 0 DEG C, and filtered, collected filtered fluid, filtered fluid and cupreol are stirred
Mix uniformly, collect stirring mixture, you can obtain Waterproof lock agent.
Example 3
The Waterproof lock agent of the present invention, includes the raw materials of following parts by weight, 42 parts of hexamethylenes, 22 parts of liquid polybutadienes, 25 parts
Acrylamide, 17 parts of glycerin monostearates, 13 parts of distilled water, 13 parts of cupreols, 5 parts of cetyltriethylammonium bromides, 4
Part gamma-aminopropyl-triethoxy-silane, 3 parts of ammonium persulfates, 0.5 part of ammonium metavanadate, 0.7 part of neodymia.
The mean molecule quantity of liquid polybutadiene in raw material is 6000.（The production of Shanghai Dong Hu Industrial Co., Ltd.s, type
Number it is Polyvest130）
The preparation of Waterproof lock agent of the present invention comprises the following steps：
（1）Match in parts by weight, take raw material；
（2）Acrylamide, distilled water, glycerin monostearate and cetyltriethylammonium bromide are put into mixer, with
900r/min is stirred 30min, collects stirring mixture, obtains emulsion；
（3）Emulsion, hexamethylene, liquid polybutadiene, ammonium metavanadate and neodymia are put into reactor, protected using nitrogen
Shield, and 0.4MPa is boosted to, preheating 15min is stirred with 200r/min at 60 DEG C, adds ammonium persulfate, stirs 35min；
（4）After stirring terminates, 105 DEG C are warming up to, stirring reaction 12h, is cooled to 75 DEG C, add the ethoxy of γ-aminopropyl three
Base silane, stir, stand 9h, be cooled to room temperature, collect reactant mixture；
（5）Reactant mixture is put into distilling apparatus, is evaporated under reduced pressure, pressure 0.04MPa, removes distilled water and hexamethylene
Alkane, distillation residue is collected, and filtered, collected filtered fluid, filtered fluid and cupreol are stirred, it is mixed to collect stirring
Compound, you can obtain Waterproof lock agent.
Example 4
The Waterproof lock agent of the present invention, includes the raw materials of following parts by weight, 40 parts of hexamethylenes, 25 parts of liquid polybutadienes, 26 parts
Acrylamide, 17 parts of glycerin monostearates, 13 parts of distilled water, 12 parts of cupreols, 5 parts of cetyltriethylammonium bromides, 4
Part gamma-aminopropyl-triethoxy-silane, 3 parts of ammonium persulfates, 0.5 part of ammonium metavanadate, 0.6 part of neodymia.
The mean molecule quantity of liquid polybutadiene in raw material is 6000.（The production of Shanghai Dong Hu Industrial Co., Ltd.s, type
Number it is Polyvest110）
The preparation of Waterproof lock agent of the present invention comprises the following steps：
（1）Match in parts by weight, take raw material；
（2）Acrylamide, distilled water, glycerin monostearate and cetyltriethylammonium bromide are put into mixer, with
900r/min is stirred 30min, collects stirring mixture, obtains emulsion；
（3）Emulsion, hexamethylene, liquid polybutadiene, ammonium metavanadate and neodymia are put into reactor, protected using nitrogen
Shield, and 0.4MPa is boosted to, preheating 15min is stirred with 200r/min at 60 DEG C, adds ammonium persulfate, stirs 35min；
（4）After stirring terminates, 105 DEG C are warming up to, stirring reaction 12h, is cooled to 75 DEG C, add the ethoxy of γ-aminopropyl three
Base silane, stir, stand 9h, be cooled to room temperature, collect reactant mixture；
（5）Reactant mixture is put into distilling apparatus, is evaporated under reduced pressure, pressure 0.04MPa, removes distilled water and hexamethylene
Alkane, distillation residue is collected, is stood overnight at 0 DEG C, and filtered, collected filtered fluid, filtered fluid and cupreol are stirred
Mix uniformly, collect stirring mixture, you can obtain Waterproof lock agent.
Reference examples 1：The Waterproof lock agent of Dongying City Co., Ltd production；
Reference examples 2：Surfactant A BS.
The Waterproof lock agent of example and reference examples is tested, specific test is as follows：
The Waterproof lock agent of example and reference examples is configured to the aqueous solution that mass fraction is 1%, in room temperature（25℃）Under use DSA-
100 surface tension instruments determine its surface tension（With distilled water）, its interfacial tension is determined with TX500-C type ultralow interfacial tension instrument
（With hexadecane）.
Its testing result such as table 1.
Table 1
| Test event | Example 1 | Example 2 | Example 3 | Example 4 | Reference examples 1 | Reference examples 2（ABS） |
| Surface tension（mN/m） | 19.5 | 18.7 | 18.9 | 19.2 | 22.6 | 23.3 |
| Interfacial tension（mN/m） | 0.34 | 0.32 | 0.33 | 0.31 | 0.45 | 0.49 |
As shown in Table 1, the Waterproof lock agent that prepared by the present invention can effectively reduce surface tension and the interfacial tension of profit, help to carry
High oil, gas phase permeability.
Claims (4)
1. a kind of Waterproof lock agent, it is characterised in that include the raw material of following parts by weight, 40~45 parts of hexamethylenes, 21~25 parts
Liquid polybutadiene, 20~28 parts of acrylamides, 15~20 parts of glycerin monostearates, 12~14 parts of distilled water, 10~15 parts
Cupreol, 4~6 parts of cetyltriethylammonium bromides, 3~5 parts of gamma-aminopropyl-triethoxy-silanes, 2~3 parts of persulfuric acid
Ammonium, 0.4~0.6 part of ammonium metavanadate, 0.1~0.8 part of neodymia.
2. Waterproof lock agent according to claim 1, it is characterised in that the mean molecule quantity of described liquid polybutadiene is
4000~10000.
3. a kind of preparation method of Waterproof lock agent as claimed in claim 1, it is characterised in that comprise the following steps：
（1）Match in parts by weight, take raw material；
（2）Acrylamide, distilled water, glycerin monostearate and cetyltriethylammonium bromide are put into mixer and carried out
Stirring, stirring mixture is collected, obtains emulsion；
（3）Emulsion, hexamethylene, liquid polybutadiene, ammonium metavanadate and neodymia are put into reactor, protected using nitrogen
Shield, is preheated at 50~60 DEG C, adds ammonium persulfate, is stirred；
（4）After stirring terminate, 90~105 DEG C are warming up to, stirring reaction, gamma-aminopropyl-triethoxy-silane is added after cooling,
Stir, stand 6~9h, be cooled to room temperature, collect reactant mixture；
（5）Reactant mixture is evaporated under reduced pressure, removes distilled water and hexamethylene, collects distillation residue, and is filtered,
Filtered fluid is collected, filtered fluid and cupreol are stirred, collects stirring mixture, you can obtain Waterproof lock agent.
4. the preparation method of Waterproof lock agent according to claim 3, it is characterised in that the step（4）In be cooled to temperature
Spend for 70~75 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710510691.3A CN107345129A (en) | 2017-06-28 | 2017-06-28 | A kind of Waterproof lock agent and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710510691.3A CN107345129A (en) | 2017-06-28 | 2017-06-28 | A kind of Waterproof lock agent and preparation method thereof |
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| Publication Number | Publication Date |
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| CN107345129A true CN107345129A (en) | 2017-11-14 |
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| CN201710510691.3A Withdrawn CN107345129A (en) | 2017-06-28 | 2017-06-28 | A kind of Waterproof lock agent and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108485616A (en) * | 2018-03-26 | 2018-09-04 | 中国石油天然气集团有限公司 | A kind of drilling fluid environment-friendly type organosilicon Waterproof lock agent and its preparation method and application |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102618224A (en) * | 2011-01-31 | 2012-08-01 | 中国石油化工集团公司 | Waterproof locking agent used for drilling fluid |
| CN102634324A (en) * | 2012-03-27 | 2012-08-15 | 中国石油大学(华东) | Waterproof locking agent for oil field and preparation method thereof |
| CN102887974A (en) * | 2012-08-14 | 2013-01-23 | 蒋官澄 | Anti-water-blocking agent for drilling fluid and preparation method thereof |
-
2017
- 2017-06-28 CN CN201710510691.3A patent/CN107345129A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102618224A (en) * | 2011-01-31 | 2012-08-01 | 中国石油化工集团公司 | Waterproof locking agent used for drilling fluid |
| CN102634324A (en) * | 2012-03-27 | 2012-08-15 | 中国石油大学(华东) | Waterproof locking agent for oil field and preparation method thereof |
| CN102887974A (en) * | 2012-08-14 | 2013-01-23 | 蒋官澄 | Anti-water-blocking agent for drilling fluid and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108485616A (en) * | 2018-03-26 | 2018-09-04 | 中国石油天然气集团有限公司 | A kind of drilling fluid environment-friendly type organosilicon Waterproof lock agent and its preparation method and application |
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Application publication date: 20171114 |