CN112010987B - Inorganic modified starch filtrate reducer for drilling fluid and preparation method thereof - Google Patents
Inorganic modified starch filtrate reducer for drilling fluid and preparation method thereof Download PDFInfo
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- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/02—Esters
- C08B31/06—Esters of inorganic acids
- C08B31/066—Starch phosphates, e.g. phosphorylated starch
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- 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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Abstract
The invention discloses an inorganic modified starch fluid loss additive for drilling fluid and a preparation method thereof, wherein the fluid loss additive takes starch as a matrix, and starch is subjected to esterification modification through sodium trimetaphosphate, so that the internal ether bond of the starch is protected, the thermal stability of the molecular structure of the starch is improved, and the temperature resistance of the product can reach 140 ℃; then, phosphate groups are introduced in the esterification process, so that the water-soluble dispersibility of the molecular chain is improved, but the molecular chain is not substantially increased, and the low viscosity effect of the drilling fluid is still kept; in addition, the modified product is subjected to pre-gelatinization treatment, so that the defect that the conventional phosphate starch has no fluid loss effect at room temperature is overcome; the inorganic modified starch fluid loss additive for the drilling fluid has the advantages of temperature resistance, fluid loss reduction performance and viscosity reduction performance, good biodegradability, capability of meeting the production environment-friendly requirement, simple and feasible corresponding preparation method steps, low cost and suitability for large-scale production.
Description
Technical Field
The invention relates to the technical field of petroleum and natural gas, in particular to an inorganic modified starch fluid loss additive for drilling fluid and a preparation method thereof.
Background
Starch has been widely used as a fluid loss additive for drilling fluid, wherein pregelatinized starch, carboxymethyl starch and graft modified starch are widely used in fluid loss additives for drilling fluid; however, among the above common starches, the pregelatinized starch has a temperature resistance of only 100 ℃, and is easily fermented in the field use process due to only physical modification, which causes the viscosity of the drilling fluid to increase and the filtration loss to increase; the temperature resistance of the carboxymethyl starch is only 120 ℃, the problem of limited use scale is also caused by the temperature resistance limit of the carboxymethyl starch, and the common carboxymethyl starch also has higher viscosity effect; although the polymer graft modified starch can effectively improve the temperature resistance, the graft comonomer can reduce the biodegradability of the starch, so that the environmental protection performance advantage is reduced, and the viscosity effect of the starch can be improved after the polymer is modified.
Disclosure of Invention
The invention aims to provide a preparation method of an inorganic modified starch fluid loss additive for drilling fluid, which has temperature resistance, fluid loss reduction performance and low viscosity.
The invention also aims to provide the inorganic modified starch fluid loss additive for the drilling fluid, which is prepared by the preparation method.
Therefore, the technical scheme of the invention is as follows:
a preparation method of an inorganic modified starch fluid loss additive for drilling fluid is characterized by comprising the following steps:
s1, dispersing starch into deionized water to obtain a starch suspension, and adjusting the pH value of the starch suspension to 7;
s2, heating the starch suspension to 40 ℃, adding sodium trimetaphosphate, and reacting for 4 hours at 40 ℃ under stirring;
s3, continuously adding acetic anhydride into the reaction liquid obtained in the step S2, and continuously reacting for 4 hours at 40 ℃ under stirring; and adjusting the pH value of the reaction product liquid to 7 after the reaction is finished;
s4, removing the solvent in the reaction product liquid by rotary evaporation, and drying and crushing the obtained solid product;
s5, carrying out high-temperature pre-gelatinization treatment on the solid particles obtained in the step S4 to obtain a product, namely the modified starch fluid loss additive; wherein, the conditions of the high-temperature pre-gelatinization treatment are as follows: deionized water in an amount of 3 wt% of the solid particles was added to the solid particles, followed by extrusion-puffing at 140 deg.C under 0.25MPa using a screw extruder.
Preferably, the starch is corn flour or tapioca flour.
Preferably, in step S1 and step S3, the pH of the solution is adjusted with sodium hydroxide.
Preferably, in step S1, the starch suspension is prepared by dispersing 100 parts by weight of starch in 200 parts by weight of deionized water and mixing.
Preferably, in step S2, sodium trimetaphosphate is added in an amount of 1.5 to 2 parts by weight.
Preferably, in step S3, the acetic anhydride is added in an amount of 3 to 5 parts by weight.
The inorganic modified starch fluid loss additive for the drilling fluid is prepared by the preparation method of the inorganic modified starch fluid loss additive for the drilling fluid.
Compared with the prior art, the beneficial effect of this application lies in:
(1) the starch is used as a matrix, the starch is subjected to esterification modification through sodium trimetaphosphate, the internal ether bond of the starch is protected, the thermal stability of the molecular structure of the starch is improved, and the temperature resistance of the product can reach 140 ℃; then, phosphate groups are introduced in the esterification process, so that the water-soluble dispersibility of the molecular chain is improved, but the molecular chain is not substantially increased, and the low viscosity effect of the drilling fluid is still kept; in addition, the modified product is subjected to pre-gelatinization treatment, so that the defect that the conventional phosphate starch has no fluid loss effect at room temperature is overcome;
(2) the inorganic modified starch fluid loss agent prepared by the preparation method has the advantages of temperature resistance, fluid loss reduction performance and viscosity reduction performance, and good biodegradability, and meets the requirement of production environmental protection;
(3) the preparation method of the inorganic modified starch fluid loss additive for the drilling fluid is simple, easy to operate, low in cost and suitable for large-scale production.
Detailed Description
The present invention will be further described with reference to the following examples, which are not intended to limit the invention in any way.
Example 1
A preparation method of an inorganic modified starch fluid loss additive for drilling fluid comprises the following steps:
s1, dispersing 100 parts by weight of corn starch into 200 parts by weight of deionized water to obtain a starch suspension, and adding sodium hydroxide to adjust the pH value of the starch suspension to 7;
s2, heating the starch suspension to 40 ℃, adding 1.5 parts by weight of sodium trimetaphosphate, and reacting for 4 hours at 40 ℃ under stirring;
s3, continuously adding 3 parts by weight of acetic anhydride into the reaction liquid obtained in the step S2, and continuously reacting for 4 hours at 40 ℃ under stirring; adding sodium hydroxide after the reaction is finished to adjust the pH value of the reaction product liquid to 7;
s4, removing the solvent in the reaction product liquid by rotary evaporation, and drying and crushing the obtained solid product;
s5, adding deionized water with the weight being 3% of the weight of the solid particles into the solid particles obtained in the step S4, and then carrying out extrusion and expansion by adopting a screw rod expander at the temperature of 140 ℃ and under the pressure of 0.25Mpa to finish the high-temperature pre-gelatinization treatment of the modified starch, wherein the obtained product is the modified starch fluid loss additive.
Example 2
A preparation method of an inorganic modified starch fluid loss additive for drilling fluid comprises the following steps:
s1, dispersing 100 parts by weight of corn starch into 200 parts by weight of deionized water to obtain a starch suspension, and adding sodium hydroxide to adjust the pH value of the starch suspension to 7;
s2, heating the starch suspension to 40 ℃, adding 2 parts by weight of sodium trimetaphosphate, and reacting for 4 hours at 40 ℃ under stirring;
s3, continuously adding 5 parts by weight of acetic anhydride into the reaction liquid obtained in the step S2, and continuously reacting for 4 hours at 40 ℃ under stirring; adding sodium hydroxide after the reaction is finished to adjust the pH value of the reaction product liquid to 7;
s4, removing the solvent in the reaction product liquid by rotary evaporation, and drying and crushing the obtained solid product;
s5, adding deionized water with the weight being 3% of the weight of the solid particles into the solid particles obtained in the step S4, and then carrying out extrusion and expansion by adopting a screw rod expander at the temperature of 140 ℃ and under the pressure of 0.25Mpa to finish the high-temperature pre-gelatinization treatment of the modified starch, wherein the obtained product is the modified starch fluid loss additive.
Example 3
A preparation method of an inorganic modified starch fluid loss additive for drilling fluid comprises the following steps:
s1, dispersing 100 parts by weight of cassava powder into 200 parts by weight of deionized water to obtain a starch suspension, and adding sodium hydroxide to adjust the pH value of the starch suspension to 7;
s2, heating the starch suspension to 40 ℃, adding 1.8 parts by weight of sodium trimetaphosphate, and reacting for 4 hours at 40 ℃ under stirring;
s3, continuously adding 4 parts by weight of acetic anhydride into the reaction liquid obtained in the step S2, and continuously reacting for 4 hours at 40 ℃ under stirring; adding sodium hydroxide after the reaction is finished to adjust the pH value of the reaction product liquid to 7;
s4, removing the solvent in the reaction product liquid by rotary evaporation, and drying and crushing the obtained solid product;
s5, adding deionized water with the weight being 3% of the weight of the solid particles into the solid particles obtained in the step S4, and then carrying out extrusion and expansion by adopting a screw rod expander at the temperature of 140 ℃ and under the pressure of 0.25Mpa to finish the high-temperature pre-gelatinization treatment of the modified starch, wherein the obtained product is the modified starch fluid loss additive.
Comparative example 1
A preparation method of an inorganic modified starch fluid loss additive for drilling fluid comprises the following steps:
s1, dispersing 100 parts by weight of corn starch into 200 parts by weight of deionized water to obtain a starch suspension, and adding sodium hydroxide to adjust the pH value of the starch suspension to 7;
s2, heating the starch suspension to 40 ℃, adding 1.5 parts by weight of sodium trimetaphosphate, and reacting for 4 hours at 40 ℃ under stirring;
s3, continuously adding 3 parts by weight of acetic anhydride into the reaction liquid obtained in the step S2, and continuously reacting for 4 hours at 40 ℃ under stirring; adding sodium hydroxide after the reaction is finished to adjust the pH value of the reaction product liquid to 7;
s4, removing the solvent in the reaction product liquid by rotary evaporation, and drying and crushing the obtained solid product to obtain the modified starch filtrate reducer.
Comparative example 2
A preparation method of an inorganic modified starch fluid loss additive for drilling fluid comprises the following steps:
s1, dispersing 100 parts by weight of corn flour into 200 parts by weight of deionized water to obtain a starch suspension, and adding sodium hydroxide to adjust the pH of the starch suspension to 7;
s2, heating the starch suspension to 40 ℃, adding 1 part by weight of sodium trimetaphosphate, and reacting for 4 hours at 40 ℃ under stirring;
s3, continuously adding 2 parts by weight of acetic anhydride into the reaction liquid obtained in the step S2, and continuously reacting for 4 hours at 40 ℃ under stirring; adding sodium hydroxide after the reaction is finished to adjust the pH value of the reaction product liquid to 7;
s4, removing the solvent in the reaction product liquid by rotary evaporation, and drying and crushing the obtained solid product;
s5, adding deionized water with the weight being 3% of the weight of the solid particles into the solid particles obtained in the step S4, and then carrying out extrusion and expansion by adopting a screw rod expander at the temperature of 140 ℃ and under the pressure of 0.25Mpa to finish the high-temperature pre-gelatinization treatment of the modified starch, wherein the obtained product is the modified starch fluid loss additive.
And (3) performance testing:
referring to GB16783.1-2014 oil and gas industry drilling fluid field test first part: water-based drilling fluid, the modified starch fluid loss additives prepared in examples 1-3 and comparative examples 1-2 were evaluated for viscosity and fluid loss performance based on 6 wt.% bentonite-based slurry. Wherein the addition amount of the modified starch fluid loss additive in the base slurry is 1.5 wt.%. The test results are shown in table 1 below.
Table 1:
from the test results in table 1, it can be seen that the modified starch fluid loss additive prepared in examples 1 to 3 shows a good fluid loss reduction effect when the addition amount of 1.5 wt.% in 6 wt.% bentonite-based slurry is 1.5 wt.%, and has substantially no obvious viscosity effect, and after curing for 16h at 140 ℃, the modified starch fluid loss additive still maintains a good fluid loss reduction effect and shows a good temperature resistance. The modified starch fluid loss additive prepared in the comparative example 1 is not subjected to pre-gelatinization treatment in the processing process, and has no fluid loss reducing effect before aging; in comparative example 2, the addition amount of the esterifying agent sodium trimetaphosphate and the addition amount of the acetic anhydride are lower than those in examples 1-3, so that the filtration loss of the fluid loss additive is obviously increased after aging at 140 ℃, namely the temperature resistance is weakened.
Biotoxicity detection was performed on examples 1-3 at a concentration of 1 wt.% with reference to SY/T6788-2010 evaluation on environmental protection technology for water-soluble oilfield chemicals. The test results are shown in table 2 below.
Table 2:
| test sample | Biotoxicity EC50(mg/L) |
| Example 1 | 1.82×106 |
| Example 2 | 1.63×106 |
| Example 3 | 1.70×106 |
As can be seen from the tests in table 2, the fluid loss additive prepared in examples 1 to 3 meets the requirements of SY/T6878-2010 "technical requirements for environmental protection of water-soluble oilfield chemicals", has no biotoxicity and good biocompatibility, and can be used in ecological environment sensitive areas.
Claims (3)
1. A preparation method of an inorganic modified starch fluid loss additive for drilling fluid is characterized by comprising the following steps:
s1, dispersing starch into deionized water to obtain a starch suspension, and adjusting the pH value of the starch suspension to 7;
in step S1, a starch suspension is prepared by dispersing 100 parts by weight of starch in 200 parts by weight of deionized water and mixing;
s2, heating the starch suspension to 40 ℃, adding sodium trimetaphosphate, and reacting for 4 hours at 40 ℃ under stirring;
in step S2, sodium trimetaphosphate is added in an amount of 1.5 to 2 parts by weight;
s3, continuously adding acetic anhydride into the reaction liquid obtained in the step S2, and continuously reacting for 4 hours at 40 ℃ under stirring; and adjusting the pH value of the reaction product liquid to 7 after the reaction is finished;
in step S3, the amount of acetic anhydride added is 3 to 5 parts by weight
S4, removing the solvent in the reaction product liquid by rotary evaporation, and drying and crushing the obtained solid product;
s5, carrying out high-temperature pre-gelatinization treatment on the solid particles obtained in the step S4, and obtaining a product which is the modified starch fluid loss additive.
2. The preparation method of the inorganic modified starch fluid loss additive for drilling fluid as claimed in claim 1, wherein the starch is corn flour or tapioca flour.
3. The inorganic modified starch fluid loss additive for drilling fluid prepared by the preparation method of the inorganic modified starch fluid loss additive for drilling fluid as claimed in any one of claims 1-2.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US5851959A (en) * | 1997-01-03 | 1998-12-22 | Chemstar Products Company | High temperature stable modified starch polymers and well drilling fluids employing same |
| CN102899005B (en) * | 2012-10-31 | 2014-03-26 | 中国石油大学(华东) | High temperature-resisting, anti-salt, anti-calcium filtrate reducer for drilling fluid and preparation method thereof |
| CN105419749A (en) * | 2015-11-18 | 2016-03-23 | 中国海洋石油总公司 | Starch filtrate reducer for drilling fluid and preparing method thereof |
| CN111057159B (en) * | 2018-10-16 | 2022-03-01 | 中国石油化工股份有限公司 | Anti-collapse modified starch for drilling fluid and preparation method thereof |
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