Disclosure of Invention
The invention aims to solve the problem that the tackifier for drilling fluid usually adopts synthetic polymer in the current low (no) solid phase drilling fluid, and has great influence on the environment, and provides a modified plantain seed husk tackifier for drilling fluid and a preparation method thereof, wherein the modified plantain seed husk tackifier has obvious viscosity improving effect in drilling fluid, is efficient and environment-friendly.
The technical scheme adopted by the invention is as follows:
the modified plantain seed husk tackifier for drilling fluid comprises the following components in percentage by mass: 31-36% of plantain seed husk, 34-35% of NaOH, 18-19% of isopropanol, 6-8% of epoxypropane, 6-8% of hydrophilic nano silicon dioxide and the balance of deionized water.
Furthermore, the particle size of the hydrophilic nano silicon dioxide is 10-50 nm.
The preparation method of the modified psyllium seed husk tackifier for drilling fluid comprises the following steps:
1) pretreatment of psyllium seed husk: washing, drying and crushing the plantain seed husk into 800-1000 meshes;
2) preparing the modified plantain seed hull tackifier for the drilling fluid: (1) adding 60-80 g of pretreated psyllium seed husk and 6-10 g of NaOH into a reactor, slowly adding 300g of distilled water, stirring at a low speed, heating to 60-80 ℃ after the NaOH is completely dissolved, and continuously stirring for reacting for 40-60 min; (2) slowly adding 20-30 g of NaOH into the reactor, slowly stirring until the NaOH is completely dissolved, slowly adding 50-80 g of water, keeping the temperature at 30-40 ℃, and continuously stirring for 15-20 min; (3) adding 30-50 g of isopropanol into the reactor in a dripping mode, keeping the temperature at 40-50 ℃ after dripping, and stirring at a low speed for 30-45 min; (4) adding 10-20 g of propylene oxide into the reactor, keeping the temperature at 40-50 ℃, and stirring at a low speed for 20-35 min; (5) adding 10-20 g of hydrophilic nano silicon dioxide into the reactor, and continuously stirring for 20-35 min; (6) removing the liquid phase of the reaction product by a vacuum filtration method, and washing by ethanol until the washing liquid is clear; (7) and drying and crushing the product to 800-1000 meshes to obtain the drilling fluid modified plantain seed husk tackifier.
Further, the drying temperature in the step (7) is 70 +/-5 ℃.
Compared with the prior art, the invention has more outstanding effects:
(1) the modified plantain seed husk tackifier for drilling fluid is synthesized by mainly adopting a solution synthesis method to form hydroxyethyl plantain seed husk, and the hydroxyethyl plantain seed husk is combined with hydrophilic nano silicon dioxide on the basis to form a hydroxyethyl plantain seed husk-nano silicon dioxide compound; (2) the psyllium seed husk is used as the main tackifier and is combined with the nano silicon dioxide, so that the tackifying effect and the temperature resistance of the system are improved; (3) compared with the current synthetic polymer, the polymer is more environment-friendly and is more suitable for being used in clay-phase-free drilling fluid, solid-phase-free drilling fluid and solid-phase-free completion fluid; (4) the method is simple, easy to implement and easy to popularize, the prepared tackifier has obvious viscosity-improving effect in the drilling fluid, the apparent viscosity of the water solution of 0.5wt% of the plantain seed husk tackifier is 22mPa.s, the temperature resistance is strong, the viscosity reduction rate of the modified plantain seed husk with the concentration of 1.0wt% is less than 30% at the temperature of 150 ℃, the treating agent has no influence on the environment, and the acute toxicity EC is50Is more than 50000, can be completely degraded and is a high-efficiency drilling fluid tackifier.
Detailed Description
The invention is further illustrated by the following examples.
The modified plantain seed husk tackifier for drilling fluid comprises the following components in percentage by mass: 31-36% of plantain seed husk, 34-35% of NaOH, 18-19% of isopropanol, 6-8% of epoxypropane, 6-8% of hydrophilic nano silicon dioxide and the balance of deionized water.
The plantain seed husk in the technical scheme of the invention is husk of dried plantain seeds, which mainly contains medicinal components such as polysaccharide compounds, iridoid, flavonoid, phenylethanoid glycoside and the like.
The particle size of the hydrophilic nano silicon dioxide is preferably 10-50 nm, the more preferably hydrophilic nano silicon dioxide is one or the combination of any two of SJ-801, SJ-1500, SJ-2500 and SJ-3500, and the product is produced by Weifang Sanjia chemical industry Co., Ltd.
The preparation method comprises the following steps:
1. pretreatment of psyllium seed husk
(1) Cleaning semen plantaginis with water, placing into oven, and drying at 100 + -5 deg.C for 5 hr;
(2) and (3) crushing the dried plantain seed husk by using a crusher, inspecting by using a standard inspection sieve, and crushing to 800-1000 meshes for later use.
2. Preparation of modified psyllium seed husk
(1) Adding 60-80 g of pretreated psyllium seed husk into a 500mL three-neck flat-bottom flask, adding 6-10 g of NaOH, slowly adding 300g of distilled water, stirring at a low speed, heating to 60-80 ℃ after NaOH is completely dissolved, and continuously stirring for reacting for 40-60 min;
(2) slowly adding 20-30 g of NaOH (flake caustic soda) into the reactor, slowly stirring until the NaOH (flake caustic soda) is completely dissolved, slowly adding 50-80 g of water, keeping the temperature at 30-40 ℃, and continuously stirring for 15-20 min;
(3) adding 30-50 g of isopropanol into the reactor in a dripping mode, keeping the temperature at 40-50 ℃ after dripping, and stirring at a low speed for 30-45 min;
(4) adding 10-20 g of propylene oxide into the reactor, keeping the temperature at 40-50 ℃, and stirring at a low speed for 20-35 min;
(5) adding 10-20 g of hydrophilic nano silicon dioxide into the reactor, and continuously stirring for 30 min;
(6) removing the liquid phase of the reaction product by a vacuum filtration method, and washing by ethanol until the washing liquid is clear;
(7) and (3) placing the product in an oven, drying at 70 +/-5 ℃, crushing the dried product by using a crusher, inspecting by using a standard inspection sieve, and crushing to 800-1000 meshes to obtain the drilling fluid modified plantain seed husk tackifier.
Example 1:
adding 60g of pretreated plantain seed husk into a 500mL three-neck flat-bottom flask, adding 6g of NaOH, slowly adding 300g of distilled water, stirring at a low speed, heating to 60 ℃ after the NaOH is completely dissolved, and continuously stirring for reacting for 40 min; slowly adding 20g NaOH (flake caustic soda), slowly stirring until all NaOH is dissolved, slowly adding 50g water, keeping the temperature at 30 ℃, and continuously stirring for 15 min; adding 30g of isopropanol in a dripping mode, and stirring at low speed for 30min while keeping the temperature at 40 ℃ after finishing dripping; adding 10g of propylene oxide, keeping the temperature at 40 ℃, and stirring at a low speed for 20 min; adding 10g of hydrophilic nano silicon dioxide SJ-801, and continuously stirring for 30 min; removing the liquid phase of the reaction product by a vacuum filtration method, and washing by ethanol until the washing liquid is clear; and (3) placing the product in an oven, drying at 70 +/-5 ℃, crushing the dried product by using a crusher, inspecting by using a standard inspection sieve, and crushing to 800-1000 meshes to obtain the drilling fluid modified plantain seed husk tackifier.
Example 2:
adding 70g of pretreated plantain seed husk into a 500mL three-neck flat-bottom flask, adding 6g of NaOH, slowly adding 300g of distilled water, stirring at a low speed, heating to 70 ℃ after the NaOH is completely dissolved, and continuously stirring for reacting for 50 min; slowly adding 25g NaOH (flake caustic soda), slowly stirring until all NaOH is dissolved, slowly adding 70g water, keeping the temperature at 35 ℃, and continuously stirring for 18 min; adding 40g of isopropanol in a dripping mode, and after dropwise adding, keeping the temperature at 45 ℃ and stirring at a low speed for 40 min; adding 15g of propylene oxide, keeping the temperature at 45 ℃, and stirring at a low speed for 20 min; adding 15g of hydrophilic nano silicon dioxide SJ-2500, and continuing stirring for 30 min; removing the liquid phase of the reaction product by a vacuum filtration method, and washing by ethanol until the washing liquid is clear; and (3) placing the product in an oven, drying at 70 +/-5 ℃, crushing the dried product by using a crusher, inspecting by using a standard inspection sieve, and crushing to 800-1000 meshes to obtain the drilling fluid modified plantain seed husk tackifier.
Example 3:
adding 80g of pretreated plantain seed husk into a 500mL three-neck flat-bottom flask, adding 6g of NaOH, slowly adding 300g of distilled water, stirring at a low speed, heating to 80 ℃ after the NaOH is completely dissolved, and continuously stirring for reacting for 60 min; slowly adding 30g NaOH (flake caustic soda), slowly stirring until all NaOH is dissolved, slowly adding 80g water, keeping the temperature at 40 ℃, and continuously stirring for 20 min; adding 50g of isopropanol in a dripping mode, keeping the temperature at 50 ℃ after the dripping is finished, and stirring at a low speed for 45 min; adding 20g of propylene oxide, keeping the temperature at 50 ℃, and stirring at a low speed for 30 min; adding 20g of hydrophilic nano silicon dioxide SJ-3500, and continuing stirring for 30 min; removing the liquid phase of the reaction product by a vacuum filtration method, and washing by ethanol until the washing liquid is clear; and (3) placing the product in an oven, drying at 70 +/-5 ℃, crushing the dried product by using a crusher, inspecting by using a standard inspection sieve, and crushing to 800-1000 meshes to obtain the drilling fluid modified plantain seed husk tackifier.
Performance testing
(1) Apparent viscosity test: measuring the apparent viscosity of the drilling fluid by adopting a drilling fluid common six-speed viscometer, aging the drilling fluid for 24 hours after the drilling fluid is prepared, detecting six-turn reading, and calculating the apparent viscosity of the system according to the 600-turn reading:
in the above formula: AV is the apparent viscosity, mpa.s;φ 600reading at 600 revolutions.
(2) And (3) testing the temperature resistance: adding 1.0% modified psyllium seed husk into the system, and detecting its apparent viscosity at room temperature by the method of (1) and recording as AV1Then pouring the mixture into a closed container, putting the container into a roller furnace, and rolling and aging the container for 24 hours at the temperature of 150 ℃; taking out, cooling, and detecting its apparent viscosity AV2The viscosity reduction rate was:
in the above formula: AV (Audio video)1Apparent viscosity before rolling, mpa.s; AV (Audio video)2Apparent viscosity after rolling, mpa.s; r is a viscosity decreasing rate.
(3) And (3) acute toxicity detection: according to the method for determining the acute toxicity of water quality of GB/T15441-1995 luminescent bacteria, the toxicity of the system is detected and recorded as EC50。
The test sample was modified psyllium husk tackifier from the above example and compared to 5% bentonite. The test results were as follows:
as can be seen from the results in FIG. 1, the apparent viscosities of 0.5% of the modified psyllium husk thickener were all over 22mPa.s, while the apparent viscosity of 5% bentonite was only 18mPa.s at ambient temperature and pressure, and the thickening effect of this system was significant.
The temperature resistance of the system was then examined and the results are shown in FIG. 2. After aging at 150 ℃, the viscosity reduction rate of the system is lower than 30 percent, which fully proves the viscosity maintaining effect and strong temperature resistance of the modified psyllium seed husk tackifier.
Finally, the acute toxicity of the three examples was examined, and from the results, the EC of the three examples was obtained50The values are 60000ppm, 65000ppm and 63000ppm, respectively, and are all non-toxic.