CN106117462A - A kind of preparation method of cement filter loss-reducing agent for oil well - Google Patents
A kind of preparation method of cement filter loss-reducing agent for oil well Download PDFInfo
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- CN106117462A CN106117462A CN201610440201.2A CN201610440201A CN106117462A CN 106117462 A CN106117462 A CN 106117462A CN 201610440201 A CN201610440201 A CN 201610440201A CN 106117462 A CN106117462 A CN 106117462A
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- reducing agent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F289/00—Macromolecular compounds obtained by polymerising monomers on to macromolecular compounds not provided for in groups C08F251/00 - C08F287/00
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
- C08F4/40—Redox systems
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
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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
- C09K8/035—Organic additives
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- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
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- General Life Sciences & Earth Sciences (AREA)
- Graft Or Block Polymers (AREA)
Abstract
The present invention is the preparation method of a kind of cement filter loss-reducing agent for oil well, comprises the following steps: lignin dissolution in deionized water, is added redox initiator Ferrous ammonium sulfate and hydrogen peroxide, is passed through nitrogen by (1), causes；(2) weighing acrylic acid and two kinds of anionic monomers of vinyl sodium benzosulfonate, being dissolved in the water and regulating pH is 6～7, and addition potassium peroxydisulfate, as initiator, is passed through nitrogen, causes；(3) lignin monomer after causing and two kinds of anionic monomer mixing, add aluminium citrate cross-linking agent and be continually fed into nitrogen, carrying out graft modification；(4), after reaction is fully completed, dehydrated alcohol, breakdown of emulsion and filtration, it is thus achieved that solid product are added.Lignin macromole is caused respectively by the present invention with modified monomer, improves the percent grafting of polyreaction, uses aluminium citrate as cross-linking agent, stable, be conducive to producing high-quality product, the inventive method is simple, can be the highest for multiple grafted monomers, feasibility.
Description
Technical field
The present invention relates to deep-well petroleum drilling fluid field, particularly relate to the preparation method of a kind of cement filter loss-reducing agent for oil well.
Background technology
In industrial propagation process, energy demand is continued to increase with China economy, domestic petroleum resources are surveyed
Visit and exploitation also deepens continuously.High temperature resistant fluid loss additive is as the important process agent in deep-well petroleum drilling fluid, and it can reduce brill
The filter loss of well liquid, ensures being smoothed out of oil extraction process, the always emphasis in oil field chemical research field.And it is wooden
Quality is as the Main By product in natural macromolecular material second largest in nature, and paper-making industry production, its reasonable development
Problem of environmental pollution will be solved greatly with utilizing, create the economic benefit with sustainable development.Traditional with lignin
Prepare, for monomer, a kind of method that the method for fluid loss additive typically refers to propose for scheme, operate comparatively laborious, use
The usual stability of cross-linking agent the highest, it may occur that dehydration and deposited phenomenon, be unfavorable for the quality of fluid loss additive product.
Summary of the invention
Present invention seek to address that the deficiencies in the prior art, and the preparation method of a kind of cement filter loss-reducing agent for oil well is provided.
The present invention for achieving the above object, by the following technical solutions: the preparation method of a kind of cement filter loss-reducing agent for oil well,
Comprise the following steps:
(1) weigh 2-5g lignin dissolution in deionized water, add redox initiator Ferrous ammonium sulfate and dioxygen
Water, the concentration of Ferrous ammonium sulfate is 0.64 × 10-4-2.56×10-4Mol/g, is passed through nitrogen, causes 15-under the conditions of 50 DEG C
30min；
(2) weigh acrylic acid and two kinds of anionic monomers of vinyl sodium benzosulfonate that ratio is 4:1-4:3, be dissolved in water
In and to regulate pH be 6～7, add potassium peroxydisulfate as initiator, the concentration of potassium peroxydisulfate is 1.85 × 10-5-7.40×10- 5Mol/g, is passed through nitrogen, causes 15～20min under the conditions of 50 DEG C；
(3) lignin monomer and two kinds of anionic monomers after causing mix, and add aluminium citrate cross-linking agent
And it is continually fed into nitrogen, it is warming up to 55-65 DEG C, in the environment of continuously stirred, react 4-6h, carry out graft modification；
(4) after reaction is fully completed, the aqueous phase solution of product is fallen in beaker, add dehydrated alcohol, by broken
Breast and filtration, it is thus achieved that khaki solid product, be placed in the baking oven of 60 DEG C and dry the powdery product obtaining being dried.
The preparation method of described aluminium citrate cross-linking agent is as follows:
(1) nitromethane solution is joined 250ml ground conical flask, put in water bath with thermostatic control, heat up and be maintained at 30
DEG C, adding anhydrous Aluminum chloride pressed powder, stirring to aluminum chloride is completely dissolved, then adds citric acid powder in solution by several times,
Strengthen stirring dynamics；
(2) ground conical flask reaction unit is transferred in vacuum distillation apparatus, distill out organic solvent nitromethane, first
Set vapo(u)rizing temperature to distill as 40 DEG C, then rise to 80 DEG C and the nitromethane in reaction system is distilled dry, finally will produce
Thing is put into vacuum drying box and is dried.
The two kinds of monomers carrying out graft modification with described lignin monomer can be acrylamide and acrylic acid.
The two kinds of monomers carrying out graft modification with described lignin monomer can be acrylamide and 2-acrylamide-2-first
Base propane sulfonic acid.
The invention has the beneficial effects as follows: the present invention carries out the synthesis of fluid loss additive with lignin for starting monomer, by wooden
Element macromole causes respectively with modified monomer, and for the Ferrous ammonium sulfate initiator selected by lignin to used by monomer
Initiator potassium persulfate has catalytic action, improves the percent grafting of polyreaction, uses aluminium citrate as cross-linking agent, stablizes,
Being conducive to producing high-quality product, the inventive method is simple, can be the highest for multiple grafted monomers, feasibility.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1: the preparation method of a kind of cement filter loss-reducing agent for oil well, comprises the following steps:
(1) weigh 2g lignin dissolution in deionized water, add redox initiator Ferrous ammonium sulfate and hydrogen peroxide,
The concentration of Ferrous ammonium sulfate is 0.64 × 10-4Mol/g, is passed through nitrogen, causes 15min under the conditions of 50 DEG C；
(2) weigh acrylic acid and two kinds of anionic monomers of vinyl sodium benzosulfonate that ratio is 4:1, be dissolved in the water also
Regulation pH is 6, and addition potassium peroxydisulfate is as initiator, and the concentration of potassium peroxydisulfate is 1.85 × 10-5Mol/g, is passed through nitrogen, 50
15min is caused under the conditions of DEG C；
(3) lignin monomer and two kinds of anionic monomers after causing mix, and add aluminium citrate cross-linking agent
And it is continually fed into nitrogen, it is warming up to 55 DEG C, in the environment of continuously stirred, react 4h, carry out graft modification；
(4) after reaction is fully completed, the aqueous phase solution of product is fallen in beaker, add dehydrated alcohol, by broken
Breast and filtration, it is thus achieved that khaki solid product, be placed in the baking oven of 60 DEG C and dry the powdery product obtaining being dried.
The preparation method of described aluminium citrate cross-linking agent is as follows:
(1) nitromethane solution is joined 250ml ground conical flask, put in water bath with thermostatic control, heat up and be maintained at 30
DEG C, adding anhydrous Aluminum chloride pressed powder, stirring to aluminum chloride is completely dissolved, then adds citric acid powder in solution by several times,
Strengthen stirring dynamics；
(2) ground conical flask reaction unit is transferred in vacuum distillation apparatus, distill out organic solvent nitromethane, first
Set vapo(u)rizing temperature to distill as 40 DEG C, then rise to 80 DEG C and the nitromethane in reaction system is distilled dry, finally will produce
Thing is put into vacuum drying box and is dried.
The two kinds of monomers carrying out graft modification with described lignin monomer can be acrylamide and acrylic acid.
The two kinds of monomers carrying out graft modification with described lignin monomer can be acrylamide and 2-acrylamide-2-first
Base propane sulfonic acid.
Embodiment 2: the preparation method of a kind of cement filter loss-reducing agent for oil well, comprises the following steps:
(1) weigh 5g lignin dissolution in deionized water, add redox initiator Ferrous ammonium sulfate and hydrogen peroxide,
The concentration of Ferrous ammonium sulfate is 2.56 × 10-4Mol/g, is passed through nitrogen, causes 30min under the conditions of 50 DEG C；
(2) weigh acrylic acid and two kinds of anionic monomers of vinyl sodium benzosulfonate that ratio is 4:3, be dissolved in the water also
Regulation pH is 7, and addition potassium peroxydisulfate is as initiator, and the concentration of potassium peroxydisulfate is 7.40 × 10-5Mol/g, is passed through nitrogen, 50
20min is caused under the conditions of DEG C；
(3) lignin monomer and two kinds of anionic monomers after causing mix, and add aluminium citrate cross-linking agent
And it is continually fed into nitrogen, it is warming up to 65 DEG C, in the environment of continuously stirred, react 6h, carry out graft modification；
(4) after reaction is fully completed, the aqueous phase solution of product is fallen in beaker, add dehydrated alcohol, by broken
Breast and filtration, it is thus achieved that khaki solid product, be placed in the baking oven of 60 DEG C and dry the powdery product obtaining being dried.
The preparation method of described aluminium citrate cross-linking agent is as follows:
(1) nitromethane solution is joined 250ml ground conical flask, put in water bath with thermostatic control, heat up and be maintained at 30
DEG C, adding anhydrous Aluminum chloride pressed powder, stirring to aluminum chloride is completely dissolved, then adds citric acid powder in solution by several times,
Strengthen stirring dynamics；
(2) ground conical flask reaction unit is transferred in vacuum distillation apparatus, distill out organic solvent nitromethane, first
Set vapo(u)rizing temperature to distill as 40 DEG C, then rise to 80 DEG C and the nitromethane in reaction system is distilled dry, finally will produce
Thing is put into vacuum drying box and is dried.
The two kinds of monomers carrying out graft modification with described lignin monomer can be acrylamide and acrylic acid.
The two kinds of monomers carrying out graft modification with described lignin monomer can be acrylamide and 2-acrylamide-2-first
Base propane sulfonic acid.
Embodiment 3: the preparation method of a kind of cement filter loss-reducing agent for oil well, comprises the following steps:
(1) weigh 3g lignin dissolution in deionized water, add redox initiator Ferrous ammonium sulfate and hydrogen peroxide,
The concentration of Ferrous ammonium sulfate is 1.92 × 10-4Mol/g, is passed through nitrogen, causes 20min under the conditions of 50 DEG C；
(2) weigh acrylic acid and two kinds of anionic monomers of vinyl sodium benzosulfonate that ratio is 4:2, be dissolved in the water also
Regulation pH is 7, and addition potassium peroxydisulfate is as initiator, and the concentration of potassium peroxydisulfate is 3.70 × 10-5Mol/g, is passed through nitrogen, 50
18min is caused under the conditions of DEG C；
(3) lignin monomer and two kinds of anionic monomers after causing mix, and add aluminium citrate cross-linking agent
And it is continually fed into nitrogen, it is warming up to 60 DEG C, in the environment of continuously stirred, react 5h, carry out graft modification；
(4) after reaction is fully completed, the aqueous phase solution of product is fallen in beaker, add dehydrated alcohol, by broken
Breast and filtration, it is thus achieved that khaki solid product, be placed in the baking oven of 60 DEG C and dry the powdery product obtaining being dried.
The preparation method of described aluminium citrate cross-linking agent is as follows:
(1) nitromethane solution is joined 250ml ground conical flask, put in water bath with thermostatic control, heat up and be maintained at 30
DEG C, adding anhydrous Aluminum chloride pressed powder, stirring to aluminum chloride is completely dissolved, then adds citric acid powder in solution by several times,
Strengthen stirring dynamics；
(2) ground conical flask reaction unit is transferred in vacuum distillation apparatus, distill out organic solvent nitromethane, first
Set vapo(u)rizing temperature to distill as 40 DEG C, then rise to 80 DEG C and the nitromethane in reaction system is distilled dry, finally will produce
Thing is put into vacuum drying box and is dried.
The two kinds of monomers carrying out graft modification with described lignin monomer can be acrylamide and acrylic acid.
The two kinds of monomers carrying out graft modification with described lignin monomer can be acrylamide and 2-acrylamide-2-first
Base propane sulfonic acid.
The present invention carries out the synthesis of fluid loss additive with lignin for starting monomer, is divided with modified monomer by lignin macromole
Do not cause, and for the Ferrous ammonium sulfate initiator selected by lignin, the initiator potassium persulfate used by monomer is had catalysis
Effect, improves the percent grafting of polyreaction, uses aluminium citrate as cross-linking agent, is in metastable shape at normal temperatures
State, does not discharge and is crosslinked with effective constituent.It is crosslinked with effective constituent when temperature is increased to certain temperature range just to slowly release, by
Gradually crosslink reaction.Due to crosslinking composition progressively discharge, the concentration in gelling solution is gradually increased, cross-linking reaction by
Progressive row, viscosity build is the slowest.When the concentration being crosslinked with effective constituent in reaction system reaches certain value, cross-linking reaction becomes bright
Show, gradually form and there is cancellated gel, can effectively block high permeability zone, produce deep profile controlling effect.This
Bright method is simple, can be the highest for multiple grafted monomers, feasibility.
Above the present invention is exemplarily described, it is clear that the present invention implements and is not subject to the restrictions described above,
As long as have employed method design and the various improvement that carry out of technical scheme of the present invention, or the most improved directly apply to other
Close, all within protection scope of the present invention.
Claims (4)
1. the preparation method of a cement filter loss-reducing agent for oil well, it is characterised in that comprise the following steps:
(1) weigh 2-5g lignin dissolution in deionized water, add redox initiator Ferrous ammonium sulfate and hydrogen peroxide, sulfur
The concentration of acid ferrous ammonium is 0.64 × 10-4-2.56×10-4Mol/g, is passed through nitrogen, causes 15-30min under the conditions of 50 DEG C；
(2) weigh acrylic acid and two kinds of anionic monomers of vinyl sodium benzosulfonate that ratio is 4:1-4:3, be dissolved in the water also
Regulation pH is 6～7, and addition potassium peroxydisulfate is as initiator, and the concentration of potassium peroxydisulfate is 1.85 × 10-5-7.40×10-5mol/
G, is passed through nitrogen, causes 15～20min under the conditions of 50 DEG C；
(3) lignin monomer and two kinds of anionic monomers after causing mix, and add aluminium citrate cross-linking agent and hold
Continue and be passed through nitrogen, be warming up to 55-65 DEG C, in the environment of continuously stirred, react 4-6h, carry out graft modification；
(4) after reaction is fully completed, the aqueous phase solution of product is fallen in beaker, adds dehydrated alcohol, by breakdown of emulsion and
Filter, it is thus achieved that khaki solid product, be placed in the baking oven of 60 DEG C and dry the powdery product obtaining being dried.
The preparation method of a kind of cement filter loss-reducing agent for oil well the most according to claim 1, it is characterised in that described citric acid
The preparation method of aluminum crosslinker is as follows:
(1) nitromethane solution is joined 250ml ground conical flask, put in water bath with thermostatic control, heat up and be maintained at 30 DEG C, adding
Entering anhydrous Aluminum chloride pressed powder, stirring to aluminum chloride is completely dissolved, then adds citric acid powder in solution by several times, and increasing is stirred
Mix dynamics；
(2) ground conical flask reaction unit is transferred in vacuum distillation apparatus, distill out organic solvent nitromethane, first set
Vapo(u)rizing temperature is 40 DEG C and distills, and then rises to 80 DEG C and is distilled by the nitromethane in reaction system dry, is finally put by product
Enter vacuum drying box to be dried.
The preparation method of a kind of cement filter loss-reducing agent for oil well the most according to claim 2, it is characterised in that wooden with described
It can be acrylamide and acrylic acid that element monomer carries out two kinds of monomers of graft modification.
The preparation method of a kind of cement filter loss-reducing agent for oil well the most according to claim 2, it is characterised in that wooden with described
It can be acrylamide and 2-acrylamide-2-methyl propane sulfonic that element monomer carries out two kinds of monomers of graft modification.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610440201.2A CN106117462A (en) | 2016-06-15 | 2016-06-15 | A kind of preparation method of cement filter loss-reducing agent for oil well |
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| CN201610440201.2A CN106117462A (en) | 2016-06-15 | 2016-06-15 | A kind of preparation method of cement filter loss-reducing agent for oil well |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106589257A (en) * | 2016-12-09 | 2017-04-26 | 孙安顺 | Preparation method of lignin grafted and copolymerized polymer flocculation type profile modifying/water plugging agent |
| CN107245132A (en) * | 2017-06-22 | 2017-10-13 | 安徽省德邦瓷业有限公司 | A kind of method that is once grafted chemical modification of sunflower seed shell lignin |
| WO2022134839A1 (en) * | 2020-12-24 | 2022-06-30 | 中国石油化工股份有限公司 | Plugging agent for oil extraction in oilfield and a preparation method therefor and application thereof |
-
2016
- 2016-06-15 CN CN201610440201.2A patent/CN106117462A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106589257A (en) * | 2016-12-09 | 2017-04-26 | 孙安顺 | Preparation method of lignin grafted and copolymerized polymer flocculation type profile modifying/water plugging agent |
| CN107245132A (en) * | 2017-06-22 | 2017-10-13 | 安徽省德邦瓷业有限公司 | A kind of method that is once grafted chemical modification of sunflower seed shell lignin |
| WO2022134839A1 (en) * | 2020-12-24 | 2022-06-30 | 中国石油化工股份有限公司 | Plugging agent for oil extraction in oilfield and a preparation method therefor and application thereof |
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