CN103289658A - Drilling fluid loss agent and preparation method thereof - Google Patents

Drilling fluid loss agent and preparation method thereof Download PDF

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Publication number
CN103289658A
CN103289658A CN2013101959726A CN201310195972A CN103289658A CN 103289658 A CN103289658 A CN 103289658A CN 2013101959726 A CN2013101959726 A CN 2013101959726A CN 201310195972 A CN201310195972 A CN 201310195972A CN 103289658 A CN103289658 A CN 103289658A
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China
Prior art keywords
drilling fluid
monomer
fluid loss
loss agent
drilling
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CN2013101959726A
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Chinese (zh)
Inventor
全红平
李欢
黄志宇
张太亮
孔权
蒋建敏
陈婷
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Southwest Petroleum University
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Southwest Petroleum University
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Priority to CN2013101959726A priority Critical patent/CN103289658A/en
Publication of CN103289658A publication Critical patent/CN103289658A/en
Pending legal-status Critical Current

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Abstract

The invention relates to a drilling fluid loss agent for oil and gas field drilling operation and a preparation method thereof. The drilling fluid loss agent is used for solving problems of short drilling liquid thickening time, large filtration loss and poor performance due to high formation temperature and large mineralization in a drilling process. The invention has the technical scheme that the drilling fluid loss agent comprises the following monomers by molar percent: 1.1-1.3% of allylpolyethyleneglycol, 82.4-86.9% of acrylamide, 12.0-16.3% of sodium p-styrenesulfonate, and ammonium persulphate served as an initiator. The preparation method comprises steps of: adding three types of monomers into the reactor; then filling water to prepare 20% solution, and utilizing 10% sodium hydroxide solution to regulate the pH value to be 9-10; and finally, filling ammonium persulfate, reacting for 3-4h at 55-60 DEG C so as to obtain a colloid product, utilizing absolute ethyl alcohol to wash until precipitate is generated, and drying in an oven at 50 DEG C so as to produce the drilling fluid loss agent. The drilling fluid loss agent has good temperature-resistant and salt-tolerance effects, is simple in preparation steps, moderate in reaction conditions and used as an oil and gas field drilling fluid additive.

Description

A kind of filtrate reducer for drilling fluid and preparation method thereof
Technical field
The present invention relates to a kind of filtrate reducer for drilling fluid for the oilfield drilling operation and preparation method thereof.
Background technology
Fluid loss agent is one for the treatment of agent the most frequently used in the oilfield drilling, and it occupies critical role in additive for drilling fluid.In drilling process, drilling fluid can cause that shale hydration expands when filter loss was excessive, caused the generation of hole instability and various complexcase, and boring the chance reservoir also can be to formation damage.The purpose that adds fluid loss agent is in order to regulate property of drilling fluid, can form thin and fine and close filter cake at the borehole wall in drilling well, reducing leak-off as far as possible to the influence on stratum.Present water-base drilling fluid fluid loss agent both domestic and external mainly is divided into natural modified high score subclass, synthetic polymer class and synthetic resin.Along with the attention of people to environment protection, some environmental protection class fluid loss agents also are exploited in addition.
Natural polymer subclass treatment agent material mainly uses Mierocrystalline cellulose, xylogen, humic acid, starch, brown coal etc., that natural materials has is cheap, the characteristics of wide material sources, therefore but heat-resisting property is generally not strong, need carry out temperature resistance, the anti-salt property that modification, grafting handle to improve product to material.
The water-soluble synthetic polymer fluid loss agent is of a great variety, is present most widely used fluid loss agent, compares with natural modified product, and synthetic base polymer has heatproof, salt tolerant, characteristics such as anti-shearing, therefore also is the emphasis of various countries researchist exploitation.Synthetic polymer class fluid loss agent is to utilize various monomers, by polyaddition reaction synthetic copolymer, terpolymer and multiple copolymer.Polyaddition reaction is the low molecular compound that contains unsaturated link(age) or ring-type, penetrates etc. in catalyzer, initiator or good fortune to add under the effect of condition, and addition mutually between monomer forms the continuous macromolecular reaction of new covalent linkage.
Synthetic polymer class fluid loss agent in R﹠D process, by choosing different reaction conditionss and different material monomer, can make product have wide in range molecular weight distribution and various functional groups owing to be to utilize various monomer addition polymerizations to form.This otherness of polymer class fluid loss agents makes this type of fluid loss agent have various over-all properties and wide application field, to satisfy the needs under the different drilling conditions.
The synthetic resin fluid loss agent is based on resol, through sulfonation or introduce other functional groups and make.The most frequently used product is sulfonated-pheno-formoldehyde resin.Such fluid loss agent is by starting monomers such as formaldehyde, phenol, obtains by polycondensation under catalyst action.Polycondensation is the monomer with two or more functional groups, and the generation macromolecular compound that reacts to each other produces the chemical reaction that simple molecules (as water, amino molecule) arranged simultaneously.
The synthetic resin fluid loss agent has the filtrate reducer for drilling fluid of good high-temperature resisting and salt-resisting filtration reduction energy, energy improvement of mud cake and stabilizing borehole.But find that in application synthetic resin fluid loss agent dosage is big, waste of raw materials is big and cause problem such as environmental pollution.
Summary of the invention
The objective of the invention is: in order to overcome in drilling process, formation temperature constantly raises along with drilling depth, and salinity constantly increases, cause the drilling fluid thickening time to shorten, filter loss increases, the problem of degradation, and the spy provides a kind of filtrate reducer for drilling fluid and preparation method thereof.
For achieving the above object, the present invention by the following technical solutions: a kind of filtrate reducer for drilling fluid is characterized in that: this filtrate reducer for drilling fluid is to be formed by allyl polyglycol and acrylamide and three kinds of monomer polymerizations of sodium p styrene sulfonate; The molar percentage of used monomer is: the allyl polyglycol monomer is 1.1~1.3%; Acrylamide monomer is 82.4~86.9%; The sodium p styrene sulfonate monomer is 12.0~16.3%; Initiator is ammonium persulphate, and add-on is 0.2~0.3% of monomer total mass.Its structural formula of this filtrate reducer for drilling fluid is as follows:
X=12.0~16.3% wherein, Y=1.1~1.3%, n=52~57.
A kind of preparation method of filtrate reducer for drilling fluid, its step are to add allyl polyglycol and the acrylamide of 0.0563mol and the sodium p styrene sulfonate of 0.0097mol of 0.00083mol earlier in reactor; It is 20% solution that the deionized water that adds 32g then in the above-mentioned monomer is mixed with the monomer mass percentage concentration, and being 10% sodium hydroxide solution with mass percentage concentration after the stirring and dissolving is adjusted to 9-10 with the pH value of reaction system; The ammonium persulphate that adds 0.016g at last, stirring in temperature is 55~60 ℃ of reaction 3-4h down, gets the colloid product, with absolute ethanol washing 3-5 time, until precipitation occurring, temperature to be deposited in is after drying by the fire 24h in 50 ℃ of baking ovens, to make this filtrate reducer for drilling fluid after the separation.The molar mass of used allyl polyglycol is 2400g/mol.
Compared with prior art, the present invention has following beneficial effect: (1) this filtrate reducer for drilling fluid preparation method step is easy, and the reaction conditions gentleness is easy to control, is used for additive for drilling fluid; (2) this filtrate reducer for drilling fluid contains nonionic long-chain polyoxyethylene groups, and it has absorption and dispersed clay particle, prevents that effectively the clay particle gathering from forming the function in leak-off duct; (3) the product thermal stability of this method preparation is better, and the temperature resistance ability is strong, and it is better to fall filtration effect in fresh water base slurry; (4) this product need not dissolution with solvents, can be directly used in the oilfield drilling liquid.
Description of drawings
Accompanying drawing is the infrared spectrum of this filtrate reducer for drilling fluid.
Embodiment
Embodiment 1
The allyl polyglycol and the acrylamide of 3.5g and the sodium p styrene sulfonate of 2g that in reactor, add 1.6g earlier; It is 20% solution that the deionized water that adds 28.4g then in the above-mentioned monomer is mixed with the monomer mass percentage concentration, being 10% sodium hydroxide solution with mass percentage concentration after the stirring and dissolving is adjusted to 9 with the pH value of reaction system, the ammonium persulphate that adds 0.0142g at last, stirring in temperature is 60 ℃ of reaction 3.5h down, get the colloid product, use absolute ethanol washing 3 times, until precipitation occurring, temperature to be deposited in is after drying by the fire 24h in 50 ℃ of baking ovens, to make this filtrate reducer for drilling fluid after the separation.
Embodiment 2
The allyl polyglycol and the acrylamide of 4g and the sodium p styrene sulfonate of 1.6g that in reactor, add 2g earlier; It is 20% solution that the deionized water that adds 30.4g then in the above-mentioned monomer is mixed with the monomer mass percentage concentration, being 10% sodium hydroxide solution with mass percentage concentration after the stirring and dissolving is adjusted to 9 with the pH value of reaction system, the ammonium persulphate that adds 0.0152g at last, stirring in temperature is 60 ℃ of reaction 4h down, get the colloid product, use absolute ethanol washing 3 times, until precipitation occurring, temperature to be deposited in is after drying by the fire 24h in 50 ℃ of baking ovens, to make this filtrate reducer for drilling fluid after the separation.
Embodiment 3
The allyl polyglycol and the acrylamide of 4g and the sodium p styrene sulfonate of 2g that in reactor, add 2g earlier; It is 20% solution that the deionized water that adds 32g then in the above-mentioned monomer is mixed with the monomer mass percentage concentration, being 10% sodium hydroxide solution with mass percentage concentration after the stirring and dissolving is adjusted to 9 with the pH value of reaction system, the ammonium persulphate that adds 0.016g at last, stirring in temperature is 60 ℃ of reaction 4h down, get the colloid product, use absolute ethanol washing 3 times, until precipitation occurring, temperature to be deposited in is after drying by the fire 24h in 50 ℃ of baking ovens, to make this filtrate reducer for drilling fluid after the separation.
Embodiment 4
The allyl polyglycol and the acrylamide of 4g and the sodium p styrene sulfonate of 2g that in reactor, add 1.8g earlier; It is 20% solution that the deionized water that adds 31.2g then in the above-mentioned monomer is mixed with the monomer mass percentage concentration, being 10% sodium hydroxide solution with mass percentage concentration after the stirring and dissolving is adjusted to 9 with the pH value of reaction system, the ammonium persulphate that adds 0.0156g at last, stirring in temperature is 60 ℃ of reaction 3.5h down, get the colloid product, use absolute ethanol washing 3 times, until precipitation occurring, temperature to be deposited in is after drying by the fire 24h in 50 ℃ of baking ovens, to make this filtrate reducer for drilling fluid after the separation.
Embodiment 5
The allyl polyglycol and the acrylamide of 4g and the sodium p styrene sulfonate of 2g that in reactor, add 2.1g earlier; It is 20% solution that the deionized water that adds 32.4g then in the above-mentioned monomer is mixed with the monomer mass percentage concentration, being 10% sodium hydroxide solution with mass percentage concentration after the stirring and dissolving is adjusted to 9 with the pH value of reaction system, the ammonium persulphate that adds 0.0162g at last, stirring in temperature is 58 ℃ of reaction 3.5h down, get the colloid product, use absolute ethanol washing 3 times, until precipitation occurring, temperature to be deposited in is after drying by the fire 24h in 50 ℃ of baking ovens, to make this filtrate reducer for drilling fluid after the separation.
Embodiment 6
Gained final product structure has been made sign with infrared spectra among the embodiment 3, and spectrogram is seen accompanying drawing, and spectrum elucidation is as follows: 1035.59cm -1The place has-SO -3Charateristic avsorption band, illustrate in the molecular structure of product and contain-SO -3Group; At 1116.58cm -1There is charateristic avsorption band at the place, illustrates and contains ether oxygen base in the product molecule; At 1670.05cm -1There is charateristic avsorption band at the place, illustrates in the product molecule and contains amide group; In addition, at 1680cm -1~1620cm -1The charateristic avsorption band of no carbon-carbon double bond illustrates and does not contain unconverted monomer in the product.
Embodiment 7
For estimating the filtration effect that falls of this fluid loss agent, at first according to GB/T16783-1997 national standard configuration base slurry.Namely add 20g wilkinite and 1g anhydrous sodium carbonate in 500ml water, the airtight 24h that leaves standstill behind high-speed stirring 30min gets bentonite content and is 4% fresh water base slurry.Get this fresh water base slurry solution of 400ml and put into ZNS-2 type pressure filter press, measure the filter loss in the 30min under its 0.7MPa pressure; Be the filter loss of fresh water base slurry.
In the fresh water base of 400ml slurry, add the product 1 that the embodiment 1 that accounts for quality of mud fluid mark 1% obtains, after stirring all then, put into the ZNS-2 type and press filter press, measure the filter loss in the 30min under its 0.7MPa pressure, namely obtain product 1 in the filter loss of fresh water base slurry; Measure product 2 that embodiment 2 obtains, product 3 that embodiment 3 obtains, product 4 that embodiment 4 obtains, product 5 that embodiment 5 obtains respectively in the filter loss of fresh water base slurry according to above method.Experimental result is as follows:
Product falls filtration effect in the table 1 fresh water base slurry
As can be seen from Table 1, the product that adds 1% embodiment, 1~5 preparation in fresh water base slurry can make filter loss be reduced to 8.8~10.3ml by 26.8ml, illustrates that the filtrate reducer for drilling fluid of embodiment 1~5 preparation can effectively reduce fresh water base slurry filter loss.

Claims (3)

1. filtrate reducer for drilling fluid is characterized in that: this filtrate reducer for drilling fluid is to be formed by allyl polyglycol and acrylamide and three kinds of monomer polymerizations of sodium p styrene sulfonate; Used monomer and molar percentage are: the allyl polyglycol monomer is 1.1~1.3%; Acrylamide monomer is 82.4~86.9%; The sodium p styrene sulfonate monomer is 12.0~16.3%; Initiator is ammonium persulphate, and add-on is 0.2~0.3% of monomer total mass.
2. the preparation method of a filtrate reducer for drilling fluid as claimed in claim 1 is characterized in that: the allyl polyglycol and the acrylamide of 0.0563mol and the sodium p styrene sulfonate of 0.0097mol that add 0.00083mol earlier in reactor; It is 20% solution that the deionized water that adds 32g then in the above-mentioned monomer is mixed with the monomer mass percentage concentration, and being 10% sodium hydroxide solution with mass percentage concentration after the stirring and dissolving is adjusted to 9-10 with the pH value of reaction system; The ammonium persulphate that adds 0.016g at last, stirring in temperature is 55~60 ℃ of reaction 3-4h down, gets the colloid product, with absolute ethanol washing 3-5 time, until precipitation occurring, temperature to be deposited in is after drying by the fire 24h in 50 ℃ of baking ovens, to make this filtrate reducer for drilling fluid after the separation.
3. filtrate reducer for drilling fluid according to claim 1 and 2, it is characterized in that: the molar mass of described allyl polyglycol is 2400g/mol.
CN2013101959726A 2013-05-24 2013-05-24 Drilling fluid loss agent and preparation method thereof Pending CN103289658A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104263329A (en) * 2014-09-19 2015-01-07 中国石油集团渤海钻探工程有限公司 High-temperature resistant and salt-tolerance filtrate reducer for drilling fluid and preparation method thereof
CN104292398A (en) * 2014-10-16 2015-01-21 西南石油大学 Temperature-resistant salt-resistant fluid loss additive for drilling fluid and preparation method thereof
CN106432601A (en) * 2016-10-17 2017-02-22 西南石油大学 Filtrate reducer and preparation method thereof
CN106543377A (en) * 2016-07-13 2017-03-29 成都菲尔特技术开发有限公司 A kind of copolymer fluid loss agent and preparation method thereof

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US20120138300A1 (en) * 2006-11-17 2012-06-07 Windal Scott Bray Method of cementing using polymeric retarder
CN101864030A (en) * 2010-07-09 2010-10-20 成都理工大学 Method for preparing temperature-resistant anti-salt amphoteric polymer filtrate reducer
CN102585090A (en) * 2011-01-10 2012-07-18 河南金马石油科技有限责任公司 Preparation method for filtrate reducer

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104263329A (en) * 2014-09-19 2015-01-07 中国石油集团渤海钻探工程有限公司 High-temperature resistant and salt-tolerance filtrate reducer for drilling fluid and preparation method thereof
CN104292398A (en) * 2014-10-16 2015-01-21 西南石油大学 Temperature-resistant salt-resistant fluid loss additive for drilling fluid and preparation method thereof
CN106543377A (en) * 2016-07-13 2017-03-29 成都菲尔特技术开发有限公司 A kind of copolymer fluid loss agent and preparation method thereof
CN106543377B (en) * 2016-07-13 2018-12-18 成都菲尔特技术开发有限公司 A kind of copolymer fluid loss agent and preparation method thereof
CN106432601A (en) * 2016-10-17 2017-02-22 西南石油大学 Filtrate reducer and preparation method thereof
CN106432601B (en) * 2016-10-17 2019-05-31 西南石油大学 A kind of fluid loss additive and preparation method thereof

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Application publication date: 20130911