CN101591527B - High temperature resistant anti-sloughing filtrate reducer for drilling fluid and preparation method thereof - Google Patents

Abstract

The invention relates to a high temperature resistant anti-sloughing filtrate reducer for a drilling fluid and a preparation method thereof. Raw materials of the anti-sloughing filtrate reducer are an acrylamide monomer, an acrylic monomer, a cationic monomer, a cross-linking agent and an initiator. The anti-sloughing filtrate reducer is prepared by the following method: adding acrylamide, the cationic monomer and the cross-linking agent into water, and stirring the mixture evenly; and adding acrylic acid solution with a neutralization degree of between 50 and 80 wt percent and the initiator into the mixture, atomizing the obtained mixed solution into liquid drops with the diameter smaller than 100 microns, and making the liquid drops dispersed in oil phase medium with a temperature of between 50 and 70 DEG C for a polymerization reaction for 3 to 5 hours. The recovery rate of shale of the anti-sloughing filtrate reducer is improved by more than 80 percent, the API filtration loss is reduced, the heat-resistant property is improved, and the high-temperature high-pressure filtration loss is lower than 30 ml.

Description

A kind of high temperature resistant anti-sloughing filtrate reducer for drilling fluid and preparation method thereof

Technical field

The present invention relates to high temperature resistant anti-sloughing filtrate reducer for drilling fluid in the Process of Oil Well Drilling and preparation method thereof, belong to the petrochemical technology field.

Technical background

Borehole well instability is to influence the principal element that drilling well is carried out smoothly always in the drilling process, and particularly under the increasing situation of deep-well, ultra deep well, orientation well and long horizontal traverse well, it is more outstanding that the problems referred to above seem.On-the-spot normal employing adds anti-collapse dose and fluid loss agent simultaneously and addresses this problem.Now anti-collapse dose commonly used has two classes, and a class is anti-collapse dose of a shutoff class, and as pitch, paraffin and calcium carbonate superfine powder etc., such anti-collapse dose by shutoff formation pore and microfracture, reduces the free water intrusion stratum in the drilling fluid and plays the effect of stabilizing borehole; Another kind of anti-collapse dose is effectively to suppress anti-collapse dose of mud shale expansion dispersive, and such anti-collapse dose enters the stratum with the drilling fluid free water, by suppressing the effect that shale hydration in the stratum expands, disperses to play stabilizing borehole.Fluid loss agent mainly makes by protective colloid effect and keeps the fine grain content of certain proportion in the drilling fluid, the mud cake permeability reduction that drilling fluid is formed, thus the free water in the reduction drilling fluid plays the effect of stabilizing borehole to the stratum leak-off.

The existing anti-collapse dose of temperature resistance ability with fluid loss agent is generally not high, generally be no more than 180 ℃, and anti-collapse dose and fluid loss agent add simultaneously and both increased drilling fluid cost, increased working strength of workers again, make drilling fluid composition complexity simultaneously, safeguard that intractability increases.

Summary of the invention

At the deficiencies in the prior art, the invention provides a kind of high temperature resistance anti-collapse and anti-falling filtration agent and preparation method thereof.Product of the present invention falls the leak-off effect with fine when having good caving-preventing characteristic, good, free from environmental pollution with the drilling fluid compatibleness, the temperature resistance ability reaches more than 200 ℃.

Technical scheme of the present invention is as follows:

Anti-collapse and anti-falling filtration agent, in 100 mass parts, the component of raw material is: acrylamide monomer 5-10 part, Acrylic Acid Monomer 1-3 part, cationic monomer 0.5-2 part, linking agent 0.05-0.10 part, initiator 0.03-0.10 part, all the other are water.Make as follows:

Acrylamide, cationic monomer and linking agent are added in the entry, stir; Adding degree of neutralization is 50-80%wt acrylic acid solution and initiator, and the gained mixing solutions is atomized into the drop below 100 microns under 50～70 ℃ of temperature, makes it to be dispersed in the oil-phase medium polyreaction 3～5 hours.

Described cationic monomer is dimethyl diallyl ammonium chloride, methylacryoyloxyethyl trimethyl ammonium chloride or acrylyl oxy-ethyl-trimethyl salmiac.

Described linking agent is N, N '-methylene-bisacrylamide.

Described initiator is ammonium persulphate or Potassium Persulphate.

The preferred white oil of described oil-phase medium.Described white oil technical grade gets final product, and can select 5#, 7#, 10# or 15# white oil for use.

Anti-collapse and anti-falling filtration agent preparation method of the present invention adopts the dispersion suspension polymerization, and step is as follows:

A, acrylamide, cationic monomer and linking agent are added in the entry, fully dissolving stirs;

B, with in the sodium hydroxide solution of 20%wt and vinylformic acid, being neutralized to degree of neutralization is 50-80%wt;

C, the acrylic acid solution for preparing in the b step is joined in the liquid that a step prepares, add initiator;

D, with high-pressure injection method mixing solutions is atomized into 5～100 microns drop, be dispersed in 50～70 ℃ the oil-phase medium polyreaction 3～5 hours, static 2-3 hour, product precipitated from oil-phase medium, promptly got high temperature resistant anti-sloughing filtrate reducer for drilling fluid after the separation.Oil-phase medium can recycling.

The high temperature resistant anti-sloughing filtrate reducer for drilling fluid outward appearance that the method for the invention makes is white or light yellow viscous liquid, and free from extraneous odour has good dissemination in water.

The high temperature resistant anti-sloughing filtrate reducer for drilling fluid that the method for the invention makes, shale rate of recovery raising rate is greater than 80%, and inhibition is less than 0.5 relatively, API filtration reduction value greater than 10ml (150 ℃/16h), high temperature and high pre ssure filtration is lower than 30ml, and the temperature resistance ability reaches more than 200 ℃.

Embodiment

Below in conjunction with embodiment the present invention is further described, but is not limited thereto.Components contents is in weight part among each embodiment, and industrial grade white oil Fushun is contained prestige petrochemical industry sales company and sold.

Embodiment 1:

At room temperature, with 5 parts of acrylamides, 1 part of dimethyl diallyl ammonium chloride (cationic monomer), 0.03 part of initiator (ammonium persulphate) and 0.05 part of N, N '-methylene-bisacrylamide (linking agent) adds in the entry, fully dissolving, the back 2 parts of degree of neutralization of adding that stir are 70% vinylformic acid.Above-mentioned reaction solution is atomized into 5～30 microns drop with high-pressure injection method, be dispersed in 60 ℃ the 7# industrial grade white oil (oil-phase medium) polyreaction 3.5 hours, static 2 hours, product precipitated from oil-phase medium, promptly got high temperature resistant anti-sloughing filtrate reducer for drilling fluid after the separation.Its performance test results is as shown in the table.

Project	Index
		Outward appearance	Colourless viscous liquid
API filtration reduction value (150 ℃/16h), mL	12.6
		API filtration reduction value (200 ℃/16h), mL	10.3
High temperature and high pre ssure filtration (150 ℃/3.5MPa), mL	22.3
		Relative inhibition	0.32
Shale reclaims raising rate, %	89.6

The performance test methods of the high temperature resistance anti-collapse and anti-falling filtration agent that the present invention relates to is as follows:

(1) mensuration of API filtration

Prepare two parts of base slurries, measure 400mL distilled water, add 16.0g sodium bentonite and 1.0g anhydrous sodium carbonate, stir 5min with high speed agitator, take off container, scrape the wilkinite that sticks on the container, continue to stir 15min, the accumulative total churning time is 20min.Under 24 ± 3 ℃ of conditions in encloses container maintenance 24h, starch as base.

Get a copy of it and add the 8g sample, then with base slurry and application of sample slurry high-speed stirring 20min, put into digestion tank at 150 ℃ in roller process furnace (or 200 ℃) rolling 16h, taking-up is cooled to 24 ± 3 ℃, high-speed stirring 5min surveys its API filtration under 24 ± 3 ℃ of conditions by the regulation of GB/T 16783-1997.Be calculated as follows API filtration reduction value:

ΔFL＝FL ₂-FL ₁

In the formula: FL ₁--the API filtration of application of sample slurry, ml

FL ₂--the API filtration of base slurry, ml

(2) mensuration of high temperature and high pre ssure filtration

Base slurry preparation: under 24 ± 3 ℃ of conditions, by water: sodium soil: estimate soil: anhydrous sodium carbonate=100: 6: 2: 0.1 ratio preparation base is starched high-speed stirring 20min, airtight again maintenance 24h.Get the base slurry 400mL for preparing, add 12.0g sample high-speed stirring 20min, the high-temperature tank of packing into, 150 ℃ of following constant temperature heat are rolled 16h, take out cooling.High-speed stirring 5min measures (150 ℃/3.5MPa) filter loss of High Temperature High Pressure.

(3) relative inhibition

Take by weighing (105 ± 3) ℃ down the drilling fluid test of baking 4h pack in the shale expansion tube with sodium bentonite 10.00g, on pressing machine, add 4MPa pressure, and keep 5min, and take off and be installed on the shale expansion instrument, measure the expansion height that 5%KCl solution and 2% sample solution soak rock core 7h respectively.Be calculated as follows relative inhibition:

$Y=\frac{h_1}{h_2}$

In the formula: Y---relative inhibition;

h ₁---2% sample solution soaks the back rock core and expands highly, mm;

h ₂---rock core expands highly after the 5%KCl solution soaking, mm.

(4) shale reclaims the mensuration of raising rate

Take by weighing two parts on air-dry mud shale landwaste (rate of recovery in distilled water is 20～40%) sample of 50g (claim accurate to 0.1g) 6～0 purposes, be respectively charged into and contain that to add the high-temperature tank middle cover of the 5% sample aqueous solution into 350mL distilled water and 350mL tight.Put into 77 ℃ the roller stove 16h that rolls, take out cooling, pour into then in the 0.45mm standard sieve (40 order), collect and tail over landwaste in watch-glass,, take out cooling, and in air, place weighing behind the 24h at (105 ± 3) ℃ constant temperature drying 4h with after the clear water rinsing.Be calculated as follows shale and reclaim the raising rate:

$F=\frac{m_H-m_W}{m_W}\×100$

In the formula:

F---shale reclaims raising rate, %;

m _H---the landwaste quality that from sample solution, reclaims, g;

m _W---the landwaste quality that from distilled water, reclaims, g.

Embodiment 2:

At room temperature, with 7 parts of acrylamides, 1.5 parts of methylacryoyloxyethyl trimethyl ammonium chlorides (cationic monomer), 0.05 part of initiator (Potassium Persulphate) and 0.06 part of N, N '-methylene-bisacrylamide (linking agent) adds in the entry, fully dissolving, the back 1 part of degree of neutralization of adding that stirs are 70% vinylformic acid.Above-mentioned reaction solution is atomized into 10～50 microns drop with high-pressure injection method, be dispersed in 55 ℃ the 10# industrial grade white oil (oil-phase medium) polyreaction 4 hours, static 2.5 hours, product precipitated from oil-phase medium, promptly got high temperature resistant anti-sloughing filtrate reducer for drilling fluid after the separation.

Get the high temperature resistance anti-collapse and anti-falling filtration agent of method for preparing, detect its performance, the result is as shown in the table.

Project	Index
		Outward appearance	Colourless viscous liquid
API filtration reduction value (150 ℃/16h), mL	11.6
		API filtration reduction value (200 ℃/16h), mL	8.5
High temperature and high pre ssure filtration (150 ℃/3.5MPa), mL	25.2
		Relative inhibition	0.42
Shale reclaims raising rate, %	91.7

Embodiment 3:

At room temperature, with 10 parts of acrylamides, 1 part of acrylyl oxy-ethyl-trimethyl salmiac (cationic monomer), 0.07 part of initiator (ammonium persulphate) and 0.09 part of N, N '-methylene-bisacrylamide (linking agent) adds in the entry, fully dissolving, the back 0.5 part of degree of neutralization of adding that stirs are 70% vinylformic acid.Above-mentioned reaction solution is atomized into 20～60 microns drop with high-pressure injection method, be dispersed in 60 ℃ the 15# industrial grade white oil (oil-phase medium) polyreaction 5 hours, static 2 hours, product precipitated from oil-phase medium, promptly got high temperature resistant anti-sloughing filtrate reducer for drilling fluid after the separation.Performance test results is as shown in the table.

Project	Index
		Outward appearance	Colourless viscous liquid
API filtration reduction value (150 ℃/16h), mL	15.2
		API filtration reduction value (200 ℃/16h), mL	11.8
High temperature and high pre ssure filtration (150 ℃/3.5MPa), mL	26.4
		Relative inhibition	0.27
Shale reclaims raising rate, %	83.7

Claims (5)

1. anti-collapse and anti-falling filtration agent is characterized in that in 100 mass parts, the component of raw material is: acrylamide monomer 5-10 part, and Acrylic Acid Monomer 1-3 part, cationic monomer 0.5-2 part, linking agent 0.05-0.10 part, initiator 0.03-0.10 part, all the other are water; Described initiator is ammonium persulphate or Potassium Persulphate; Make as follows:

A, acrylamide, cationic monomer and linking agent are added in the entry, fully dissolving stirs;

B, with in the sodium hydroxide solution of 20%wt and vinylformic acid, being neutralized to degree of neutralization is 50-80%wt;

C, the acrylic acid solution for preparing in the b step is joined in the liquid that a step prepares, add initiator;

D, with high-pressure injection method mixing solutions is atomized into 5～100 microns drop, be dispersed in 50～70 ℃ the oil-phase medium white oil polyreaction 3～5 hours, static 2-3 hour, product precipitated from oil-phase medium, promptly got high temperature resistant anti-sloughing filtrate reducer for drilling fluid after the separation.

2. anti-collapse and anti-falling filtration agent as claimed in claim 1 is characterized in that described cationic monomer is dimethyl diallyl ammonium chloride, methylacryoyloxyethyl trimethyl ammonium chloride or acrylyl oxy-ethyl-trimethyl salmiac.

3. anti-collapse and anti-falling filtration agent as claimed in claim 1 is characterized in that described linking agent is N, N '-methylene-bisacrylamide.

4. anti-collapse and anti-falling filtration agent as claimed in claim 1 is characterized in that described white oil selects technical grade 5#, 7#, 10# or 15# white oil for use.

5. the preparation method of the described anti-collapse and anti-falling filtration agent of claim 1 adopts the dispersion suspension polymerization, and step is as follows:

A, acrylamide, cationic monomer and linking agent are added in the entry, fully dissolving stirs;

B, with in the sodium hydroxide solution of 20%wt and vinylformic acid, being neutralized to degree of neutralization is 50-80%wt;

C, the acrylic acid solution for preparing in the b step is joined in the liquid that a step prepares, add initiator;

D, with high-pressure injection method mixing solutions is atomized into 5～100 microns drop, be dispersed in 50～70 ℃ the oil-phase medium polyreaction 3～5 hours, static 2-3 hour, product precipitated from oil-phase medium, promptly got high temperature resistant anti-sloughing filtrate reducer for drilling fluid after the separation.