CN111040740A - Preparation method of persistent high-temperature-resistant salt-resistant filtrate reducer - Google Patents
Preparation method of persistent high-temperature-resistant salt-resistant filtrate reducer Download PDFInfo
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Abstract
The invention discloses a preparation method of a durable high-temperature-resistant and salt-resistant filtrate reducer, belonging to the technical field of drilling compositions. A preparation method of a durable high-temperature-resistant salt-resistant filtrate reducer comprises the following steps: 1) mixing lignite and a sodium hydroxide solution for reaction, filtering, and removing unreacted water insoluble substances to obtain a sodium humate solution for later use; 2) adding phenol, formaldehyde water solution and sodium styrene sulfonate into a reaction kettle, adding the sodium humate solution obtained in the step 1) after the reaction is finished, adding a sulfonating agent, reacting for 45-90 minutes, and drying to obtain a product. The preparation method of the fluid loss agent is greatly improved based on the traditional process, so that the purpose of greatly improving the technical performance index of the fluid loss agent is realized, the high temperature resistance and the durability are remarkably improved compared with the prior art, and the defects of large dosage, unobvious effect and the like of the fluid loss agent in the using process are overcome.
Description
Technical Field
The invention belongs to the technical field of drilling compositions, and particularly relates to a preparation method of a durable high-temperature-resistant salt-resistant filtrate reducer.
Background
With the increasing demand of industrial development for petroleum, the development of oil and gas resources stored in deep land strata, deep sea and areas with severe environment is required, which makes the drilling of deep wells and ultra-deep wells an important research direction for the development of oil and gas resources. In the drilling of deep wells and ultra-deep wells, the drilling fluid process technology is an important guarantee for realizing safe and rapid operation of the deep wells and the ultra-deep wells. In order to maintain or basically maintain the original performance of the drilling fluid under the conditions of high temperature, high pressure, high density, high salinity and the like, a novel drilling fluid treating agent suitable for drilling deep wells and ultra-deep wells needs to be developed so as to meet the production requirements of a drilling process on safety, high efficiency, environmental protection and economy. The filtrate reducer is used as an important drilling fluid treating agent, and the temperature resistance and salt resistance of the filtrate reducer directly influence the performance of the water-based drilling fluid. The purpose of adding fluid loss additives is to reduce the fluid loss of the drilling fluid as much as possible by forming a thin and dense filter cake with low permeability on the well wall. With the continuous deepening of research and the increasingly complex conditions of drilling and meeting stratum, the existing fluid loss additive cannot meet the requirements of drilling operation, so that research personnel are promoted to research and develop towards the aspect of novel high-temperature-resistant fluid loss additive.
Patent document CN 109370546A discloses a fluid loss additive AMPS-DMC copolymer TCJ-2 for drilling fluid and a preparation method thereof. The composite material is prepared from the following raw materials in parts by weight: 20-50 parts of lignite, 10-30 parts of dimethyl carbonate (DMC), 10-20 parts of AMPS, 10-25 parts of phenol, 10-20 parts of formaldehyde, 10-20 parts of sodium hydroxide, 5-20 parts of water, 5-10 parts of soda ash and 5-10 parts of cationic monomer. The product of the invention is a novel cationic high-temperature-resistant salt-resistant filtrate reducer, and can resist the temperature of more than 150 ℃ when being added into a drilling fluid system, and the salt resistance of a single agent is more than 4%. The temperature resistance and the temperature resistance durability of the fluid loss additive are both required to be further improved.
Patent document No. CN 109912757 a discloses a method for preparing a resin filtrate reducer, which comprises phenol, formaldehyde, sodium metabisulfite, sodium sulfite, propyl sulfonic acid monomer and high-temperature stabilizer, wherein the raw materials respectively comprise the following components in parts by weight: 27% -33% of phenol, 47% -55% of formaldehyde, 10% -14% of sodium metabisulfite, 5% -10% of sodium sulfite, 0.5% -0.8% of propane sulfonic acid group monomer and 0.3% -0.5% of high-temperature stabilizer. The resin filtrate reducer prepared by the preparation method has strong temperature resistance of products, can resist saturated salt and compound salt in a drilling fluid system at 220 ℃, has strong salt resistance, but has poor temperature durability and needs to be improved.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a preparation method of a filtrate reducer with lasting high temperature resistance and salt resistance, so as to improve the temperature resistance and temperature resistance lasting performance of the filtrate reducer.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of a durable high-temperature-resistant salt-resistant filtrate reducer comprises the following steps:
1) mixing lignite and a sodium hydroxide solution for reaction, filtering, and removing unreacted water insoluble substances to obtain a sodium humate solution for later use;
2) adding phenol, formaldehyde water solution and sodium styrene sulfonate into a reaction kettle, adding the sodium humate solution obtained in the step 1) after the reaction is finished, adding a sulfonating agent, reacting for 45-90 minutes, and drying to obtain a product.
Preferably, the reaction time of the lignite and the sodium hydroxide solution is 50-90 minutes.
Preferably, the mass fraction of sodium hydroxide in the sodium hydroxide solution is 30-50%.
Preferably, the reaction time of the phenol, formaldehyde and sodium styrene sulfonate is 50 to 90 minutes.
Preferably, the reaction time of the phenol, formaldehyde and sodium styrene sulfonate is 60 minutes.
Preferably, the drying is spray drying.
Preferably, the durable high-temperature-resistant salt-resistant filtrate reducer is prepared from the following raw materials in parts by weight: 20-40 parts of lignite, 10-20 parts of sodium hydroxide, 10-30 parts of phenol, 30-50 parts of formaldehyde water solution, 5-20 parts of sodium styrene sulfonate and 1-10 parts of sulfonating agent.
Preferably, the concentration of the aqueous formaldehyde solution is 30 to 35%.
Preferably sodium metabisulfite and sodium bisulfite in a weight ratio of 1: 1.
the temperature and salt resistance of the fluid loss additive directly affects the performance of the water-based drilling fluid, and the prior art (see Q/SH 0047-2007) aiming at the high temperature and salt resistance of the fluid loss additive can only achieve the following effects: (1) rolling for 16h at 180 ℃ until the high-temperature high-pressure filtration loss of the fresh water mud is less than or equal to 30ml, and (2) rolling for 16h at 180 ℃ until the high-temperature high-pressure filtration loss of the salt water mud is less than or equal to 35 ml. And for deep wells and ultra-deep wells, the bottom temperature can reach 200 ℃ or even higher. Under the high-temperature environment, the clay in the drilling fluid can be dispersed, purified and agglomerated; the filtrate reducer can be degraded and crosslinked, and can be desorbed and dehydrated on clay, and the like, which can cause the performance of the drilling fluid to be changed sharply and have important influence on the drilling process. Therefore, the research and development of a novel high-temperature resistant filtrate reducer are important problems which need to be solved urgently by oil field workers. In the existing high-temperature-resistant and salt-resistant drilling fluid system, the sulfomethyl phenolic resin needs to be compounded with sulfonated lignite SMC, lignite resin SPNH, sulfonated tannin extract SMK and the like for use to exert a good fluid loss reduction effect, but the drilling fluid system of the type is usually accompanied by phenomena of high-temperature thickening, high-salt thickening and the like, so that a plurality of problems exist in field application, such as low temperature resistance, low high-temperature-resistant durability and the like.
Compared with the prior art, the invention has the following beneficial effects:
1) the preparation method of the fluid loss agent is greatly improved based on the traditional process, so that the purpose of greatly improving the technical performance index of the fluid loss agent is realized, the high temperature resistance and the durability are remarkably improved compared with the prior art, and the defects of large dosage, unobvious effect and the like of the fluid loss agent in the using process are overcome.
2) The preparation method of the fluid loss agent refines the reaction process, on one hand, the reaction is complete, on the other hand, the influence of water insoluble substances in the lignite on the reaction is reduced, and the product performance formed by the reaction is better.
3) The filtrate reducer of the invention can resist high temperature of more than 200 ℃, and has obvious improvement on high temperature resistance compared with the existing salt-resistant and high temperature-resistant filtrate reducer.
4) The filtrate reducer of the invention rolls in a roller furnace for 36 hours at a high temperature of 200 ℃, the slurry performance is unchanged, and the high temperature durability of the filtrate reducer is obviously improved compared with the prior salt-resistant high temperature-resistant filtrate reducer.
5) The general additive amount of the filtrate reducer is about 1 percent, the additive amount is less than that of similar products, the production cost is reduced, and the using amount of slurry is reduced.
Detailed Description
In order to better understand the present invention, the following examples are further provided to clearly illustrate the contents of the present invention, but the contents of the present invention are not limited to the following examples. In the following description, numerous specific details are set forth in order to provide a more thorough understanding of the present invention.
The term "prepared from …" as used herein is synonymous with "comprising". The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
The conjunction "consisting of …" excludes any unspecified elements, steps or components. If used in a claim, the phrase is intended to claim as closed, meaning that it does not contain materials other than those described, except for the conventional impurities associated therewith. When the phrase "consisting of …" appears in a clause of the subject matter of the claims rather than immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.
The raw materials used in the invention are as follows:
A) phenol, C6H5OH, purity 99.99%;
B) formaldehyde, CHO, 30% aqueous solution;
C) sodium styrene sulfonate, C8H7O3SNa, SSS, purity 99.99%;
D) brown coal, the purity is 40%;
E) sodium hydroxide, NaOH, purity 96%;
F) sodium metabisulfite, sodium sulfite, purity 99%.
Example 1
A preparation method of a durable high-temperature-resistant salt-resistant filtrate reducer comprises the following steps:
1) mixing lignite and a sodium hydroxide solution for reacting for 60 minutes, filtering, and removing unreacted water insoluble substances to obtain a sodium humate solution for later use;
2) adding phenol, formaldehyde water solution and sodium styrene sulfonate into a reaction kettle, reacting for 60 minutes, adding the sodium humate solution obtained in the step 1), adding a sulfonating agent, reacting for 60 minutes, and drying to obtain a product.
Wherein the mass fraction of sodium hydroxide in the sodium hydroxide solution is 30%.
As a preferred embodiment of the invention, the reaction temperature of each stage is controlled to be 20-45 ℃, and circulating water is adopted to cool the temperature to the temperature range above 45 ℃ so as to ensure the effective reaction of each stage. The real-time reaction temperature of each stage may be any value within the range of 20 to 45 ℃, for example, 20 ℃, 25 ℃, 30 ℃, 35 ℃, 40 ℃, 45 ℃ and the like.
As a preferred embodiment of the present invention, the drying is spray drying, the inlet air temperature is 100-: 100 deg.C, 102 deg.C, 105 deg.C, 108 deg.C, 110 deg.C, etc., and the air outlet temperature can be selected from any temperature value between 40-50 deg.C, such as 40 deg.C, 42 deg.C, 45 deg.C, 48 deg.C, 50 deg.C, etc.
The durable high-temperature-resistant salt-resistant filtrate reducer is prepared from the following raw materials in parts by weight: 30 parts of lignite, 15 parts of sodium hydroxide, 20 parts of phenol, 40 parts of formaldehyde water solution, 12 parts of sodium styrene sulfonate and 5 parts of sulfonating agent.
The concentration of the aqueous formaldehyde solution was 30%.
The sulfonating agent is a composition of sodium metabisulfite and sodium bisulfite, and the weight ratio of the sodium metabisulfite to the sodium bisulfite is 1: 1.
example 2
A preparation method of a durable high-temperature-resistant salt-resistant filtrate reducer comprises the following steps:
1) mixing lignite and a sodium hydroxide solution for reacting for 60 minutes, filtering, and removing unreacted water insoluble substances to obtain a sodium humate solution for later use;
2) adding phenol, formaldehyde water solution and sodium styrene sulfonate into a reaction kettle, reacting for 50 minutes, adding the sodium humate solution obtained in the step 1), adding a sulfonating agent, reacting for 60 minutes, and drying to obtain a product.
Wherein the mass fraction of sodium hydroxide in the sodium hydroxide solution is 35%.
The durable high-temperature-resistant salt-resistant filtrate reducer is prepared from the following raw materials in parts by weight: 25 parts of lignite, 12 parts of sodium hydroxide, 15 parts of phenol, 35 parts of formaldehyde water solution, 8 parts of sodium styrene sulfonate and 3 parts of sulfonating agent.
The concentration of the aqueous formaldehyde solution was 32%.
The sulfonating agent is a composition of sodium metabisulfite and sodium bisulfite, and the weight ratio of the sodium metabisulfite to the sodium bisulfite is 1: 1.
example 3
A preparation method of a durable high-temperature-resistant salt-resistant filtrate reducer comprises the following steps:
1) mixing lignite and a sodium hydroxide solution for reacting for 60 minutes, filtering, and removing unreacted water insoluble substances to obtain a sodium humate solution for later use;
2) adding phenol, formaldehyde water solution and sodium styrene sulfonate into a reaction kettle, reacting for 70 minutes, adding the sodium humate solution obtained in the step 1), adding a sulfonating agent, reacting for 50 minutes, and drying to obtain a product.
Wherein the mass fraction of sodium hydroxide in the sodium hydroxide solution is 40%.
The durable high-temperature-resistant salt-resistant filtrate reducer is prepared from the following raw materials in parts by weight: 20 parts of lignite, 10 parts of sodium hydroxide, 10 parts of phenol, 30 parts of formaldehyde water solution, 5 parts of sodium styrene sulfonate and 1 part of sulfonating agent.
The concentration of the aqueous formaldehyde solution was 35%.
The sulfonating agent is a composition of sodium metabisulfite and sodium bisulfite, and the weight ratio of the sodium metabisulfite to the sodium bisulfite is 1: 1.
example 4
A preparation method of a durable high-temperature-resistant salt-resistant filtrate reducer comprises the following steps:
1) mixing lignite and a sodium hydroxide solution for reacting for 60 minutes, filtering, and removing unreacted water insoluble substances to obtain a sodium humate solution for later use;
2) adding phenol, formaldehyde water solution and sodium styrene sulfonate into a reaction kettle, reacting for 80 minutes, adding the sodium humate solution obtained in the step 1), adding a sulfonating agent, reacting for 60 minutes, and drying to obtain a product.
Wherein the mass fraction of sodium hydroxide in the sodium hydroxide solution is 45%.
The durable high-temperature-resistant salt-resistant filtrate reducer is prepared from the following raw materials in parts by weight: 35 parts of lignite, 18 parts of sodium hydroxide, 28 parts of phenol, 45 parts of formaldehyde water solution, 15 parts of sodium styrene sulfonate and 8 parts of sulfonating agent.
The concentration of the aqueous formaldehyde solution was 30%.
The sulfonating agent is a composition of sodium metabisulfite and sodium bisulfite, and the weight ratio of the sodium metabisulfite to the sodium bisulfite is 1: 1.
example 5
A preparation method of a durable high-temperature-resistant salt-resistant filtrate reducer comprises the following steps:
1) mixing lignite and a sodium hydroxide solution for reacting for 60 minutes, filtering, and removing unreacted water insoluble substances to obtain a sodium humate solution for later use;
2) adding phenol, formaldehyde water solution and sodium styrene sulfonate into a reaction kettle, reacting for 90 minutes, adding the sodium humate solution obtained in the step 1), adding a sulfonating agent, reacting for 70 minutes, and drying to obtain a product.
Wherein the mass fraction of sodium hydroxide in the sodium hydroxide solution is 50%.
The durable high-temperature-resistant salt-resistant filtrate reducer is prepared from the following raw materials in parts by weight: 40 parts of lignite, 20 parts of sodium hydroxide, 30 parts of phenol, 50 parts of formaldehyde water solution, 20 parts of sodium styrene sulfonate and 10 parts of sulfonating agent.
The concentration of the aqueous formaldehyde solution was 30%.
The sulfonating agent is a composition of sodium metabisulfite and sodium bisulfite, and the weight ratio of the sodium metabisulfite to the sodium bisulfite is 1: 1.
example 6
A preparation method of a durable high-temperature-resistant salt-resistant filtrate reducer comprises the following steps:
1) mixing lignite and a sodium hydroxide solution for reacting for 60 minutes, filtering, and removing unreacted water insoluble substances to obtain a sodium humate solution for later use;
2) adding phenol, formaldehyde water solution and sodium styrene sulfonate into a reaction kettle, reacting for 60 minutes, adding the sodium humate solution obtained in the step 1), adding a sulfonating agent, reacting for 90 minutes, and drying to obtain a product.
Wherein the mass fraction of sodium hydroxide in the sodium hydroxide solution is 35%.
The durable high-temperature-resistant salt-resistant filtrate reducer is prepared from the following raw materials in parts by weight: 23 parts of lignite, 16 parts of sodium hydroxide, 12 parts of phenol, 32 parts of formaldehyde water solution, 7 parts of sodium styrene sulfonate and 4 parts of sulfonating agent.
The concentration of the aqueous formaldehyde solution was 35%.
The sulfonating agent is a composition of sodium metabisulfite and sodium bisulfite, and the weight ratio of the sodium metabisulfite to the sodium bisulfite is 1: 1.
example 7
A preparation method of a durable high-temperature-resistant salt-resistant filtrate reducer comprises the following steps:
1) mixing lignite and a sodium hydroxide solution for reacting for 60 minutes, filtering, and removing unreacted water insoluble substances to obtain a sodium humate solution for later use;
2) adding phenol, formaldehyde water solution and sodium styrene sulfonate into a reaction kettle, reacting for 60 minutes, adding the sodium humate solution obtained in the step 1), adding a sulfonating agent, reacting for 75 minutes, and drying to obtain a product.
Wherein the mass fraction of sodium hydroxide in the sodium hydroxide solution is 40%.
The durable high-temperature-resistant salt-resistant filtrate reducer is prepared from the following raw materials in parts by weight: 38 parts of lignite, 17 parts of sodium hydroxide, 26 parts of phenol, 48 parts of a formaldehyde water solution, 18 parts of sodium styrene sulfonate and 9 parts of a sulfonating agent.
The concentration of the aqueous formaldehyde solution was 30%.
The sulfonating agent is a composition of sodium metabisulfite and sodium bisulfite, and the weight ratio of the sodium metabisulfite to the sodium bisulfite is 1: 1.
example 8
A preparation method of a durable high-temperature-resistant salt-resistant filtrate reducer comprises the following steps:
1) mixing lignite and a sodium hydroxide solution for reacting for 60 minutes, filtering, and removing unreacted water insoluble substances to obtain a sodium humate solution for later use;
2) adding phenol, formaldehyde water solution and sodium styrene sulfonate into a reaction kettle, reacting for 65 minutes, adding the sodium humate solution obtained in the step 1), adding a sulfonating agent, reacting for 85 minutes, and drying to obtain a product.
Wherein the mass fraction of sodium hydroxide in the sodium hydroxide solution is 40%.
The durable high-temperature-resistant salt-resistant filtrate reducer is prepared from the following raw materials in parts by weight: 32 parts of lignite, 19 parts of sodium hydroxide, 23 parts of phenol, 42 parts of formaldehyde water solution, 16 parts of sodium styrene sulfonate and 6 parts of sulfonating agent.
The concentration of the aqueous formaldehyde solution was 32%.
The sulfonating agent is a composition of sodium metabisulfite and sodium bisulfite, and the weight ratio of the sodium metabisulfite to the sodium bisulfite is 1: 1.
comparative example 1
This comparative example 1 differs from example 1 in that:
the preparation method of the filtrate reducer comprises the following steps: pumping phenol into a reaction kettle through a conveying sealing pump, adding a formaldehyde aqueous solution under the sealed condition, adding lignite, adjusting the pH value to 8.0, adding a sulfonating agent, reacting for 1 hour, and performing spray drying to obtain the phenol formaldehyde resin.
The spray drying conditions were the same as in inventive example 1.
Comparative example 2
This comparative example 1 differs from example 1 in that:
the step 2) is as follows: mixing the sodium humate solution obtained in the step 1) with phenol, a formaldehyde aqueous solution and sodium styrene sulfonate, adding a sulfonating agent, reacting for 85 minutes, and drying to obtain a product.
Wherein the sulfonating agent is sodium pyrosulfite.
Comparative example 3
This comparative example 1 differs from example 1 in that: the weight portion of the added sodium styrene sulfonate is 2 portions.
And (3) performance measurement:
1. the performance of the filtrate reducer prepared according to the invention and the comparative examples 1-3 is detected, the sampling standard is carried out according to GB/T6678-2003, the test method is carried out according to Q/SH 0047-2007 salt-resistant and high-temperature-resistant filtrate reducer for drilling fluid, and the test results are shown in the following table.
2. The temperature resistance and durability of the samples of the invention and the samples of the comparative examples 1 to 3 are detected by referring to a test method of a 150g/L sodium chloride pollution drilling fluid performance test in Q/SH 0047-2007 salt-resistant high-temperature-resistant fluid loss additive for drilling fluid, and the results are shown in the following table.
After the filtrate reducer of the invention rolls in a high-temperature roller furnace at 200 ℃ for 36 hours, the performance index still meets the standard requirement, and compared with comparative examples 1-3, the filtrate reducer has remarkable progress.
Finally, the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting, and other modifications or equivalent substitutions made by the technical solutions of the present invention by those of ordinary skill in the art should be covered within the scope of the claims of the present invention as long as they do not depart from the spirit and scope of the technical solutions of the present invention.
Claims (9)
1. A preparation method of a durable high-temperature-resistant salt-resistant filtrate reducer is characterized by comprising the following steps: the method comprises the following steps:
1) mixing lignite and a sodium hydroxide solution for reaction, filtering, and removing unreacted water insoluble substances to obtain a sodium humate solution for later use;
2) adding phenol, formaldehyde water solution and sodium styrene sulfonate into a reaction kettle, adding the sodium humate solution obtained in the step 1) after the reaction is finished, adding a sulfonating agent, reacting for 45-90 minutes, and drying to obtain a product.
2. The preparation method of the durable high-temperature-resistant salt-resistant fluid loss additive according to claim 1, which is characterized by comprising the following steps: the reaction time of the lignite and the sodium hydroxide solution is 50-90 minutes.
3. The preparation method of the durable high-temperature-resistant salt-resistant fluid loss additive according to claim 2, characterized by comprising the following steps: the mass fraction of sodium hydroxide in the sodium hydroxide solution is 30-50%.
4. The preparation method of the durable high-temperature-resistant salt-resistant fluid loss additive according to claim 3, characterized by comprising the following steps: the reaction time of the phenol, the formaldehyde and the sodium styrene sulfonate is 50-90 minutes.
5. The preparation method of the durable high-temperature-resistant salt-resistant fluid loss additive according to claim 4, characterized by comprising the following steps: the reaction time of the phenol, formaldehyde and sodium styrene sulfonate was 60 minutes.
6. The preparation method of the durable high-temperature-resistant salt-resistant fluid loss additive according to claim 5, characterized by comprising the following steps: the drying is spray drying.
7. The method for preparing the durable high-temperature-resistant salt-resistant fluid loss additive according to any one of claims 1 to 5, wherein the method comprises the following steps: the durable high-temperature-resistant salt-resistant filtrate reducer is prepared from the following raw materials in parts by weight: 20-40 parts of lignite, 10-20 parts of sodium hydroxide, 10-30 parts of phenol, 30-50 parts of formaldehyde water solution, 5-20 parts of sodium styrene sulfonate and 1-10 parts of sulfonating agent.
8. The preparation method of the durable high-temperature-resistant salt-resistant fluid loss additive according to claim 7, which is characterized by comprising the following steps: the concentration of the formaldehyde aqueous solution is 30-35%.
9. The preparation method of the durable high-temperature-resistant salt-resistant fluid loss additive according to claim 8, characterized in that: the sulfonating agent is sodium metabisulfite and sodium bisulfite, and the weight ratio of the sodium metabisulfite to the sodium bisulfite is 1: 1.
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Application publication date: 20200421 |