CN114106794B - Environment-friendly high-temperature-resistant filtrate reducer and preparation method thereof - Google Patents
Environment-friendly high-temperature-resistant filtrate reducer and preparation method thereof Download PDFInfo
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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
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- C09K8/03—Specific additives for general use in well-drilling compositions
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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- C08F218/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, of carbonic acid or of a haloformic acid
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- C08F220/10—Esters
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- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
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Abstract
The application relates to the technical field of drilling fluid additives, and particularly discloses an environment-friendly high-temperature-resistant fluid loss agent and a preparation method thereof, wherein the fluid loss agent is prepared from the following raw materials in parts by weight: 40-60 parts of alkyl vinyl ester monomer, 3-8 parts of emulsifier, 7-15 parts of cross-linking agent, 0.5-1.5 parts of initiator, 8-15 parts of cellulose and 20-45 parts of water; the preparation method comprises the following steps: preparing a pre-emulsion: stirring and emulsifying alkyl vinyl ester monomer, emulsifier, cross-linking agent and (1/5-2/5) water to prepare pre-emulsion; preparing a filtrate reducer: and mixing the obtained pre-emulsion with an initiator, stirring to obtain a mixed emulsion, dropwise adding the mixed emulsion into the residual water at 65-80 ℃, adding cellulose, reacting, and adjusting the pH value to alkalescence to obtain the fluid loss agent. The filtrate reducer has the characteristics of high temperature resistance, salt resistance and less influence on the environment.
Description
Technical Field
The application relates to the technical field of drilling fluid additives, in particular to an environment-friendly high-temperature-resistant fluid loss additive and a preparation method thereof.
Background
The filtration loss of the drilling fluid and the formation of a filter cake are inevitable in the drilling process, the filter cake can be formed through the filtration loss to protect the well wall, but the too large filtration loss of the drilling fluid can easily cause the shale to expand and collapse, so that the well wall is unstable. In addition, the filter cake thickens while the filtration loss is increased, so that the well diameter is reduced, a large torque is caused to a rotating drilling tool, swabbing and pressure fluctuation are caused when the drilling tool is tripped out, and differential pressure drill sticking is easily caused.
Therefore, the filtrate reducer is usually added into the drilling fluid, and the addition of the filtrate reducer can obviously reduce the filtrate loss of the drilling fluid, maintain and stabilize the well wall and ensure that the drilling is carried out quickly and safely. The existing filtrate reducers mainly comprise the following types: cellulose, humic acid, resin and starch, wherein the cellulose filtrate reducer has a wide application system range, but the viscosity of the drilling fluid is obviously improved, the cost is high, and the temperature resistance is poor, and the filtrate reducers such as the humic acid and the resin have certain temperature resistance, but the products have dark colors, and when the filtrate reducers are used for drilling, the influences on the surrounding environment are large, and the demand for providing a novel filtrate reducer which has salt resistance, high temperature resistance and smaller influences on the environment is urgent.
Disclosure of Invention
In order to obtain the filtrate reducer which is resistant to high temperature and salt and has less influence on the environment, the application provides an environment-friendly high-temperature resistant filtrate reducer and a preparation method thereof.
The application provides an environment-friendly high temperature resistant filtrate reducer adopts the following technical scheme:
an environment-friendly high-temperature resistant filtrate reducer is prepared from the following raw materials in parts by weight:
40-60 parts of alkyl vinyl ester monomer, 3-8 parts of emulsifier, 7-15 parts of cross-linking agent, 0.5-1.5 parts of initiator, 8-15 parts of cellulose and 20-45 parts of water.
By adopting the technical scheme, the hydroxyl on the cellulose polymer chain and the oxygen atoms on the surface of the clay particles form hydrogen bond adsorption, electrostatic attraction is generated between part of hydroxyl and aluminum ions at the edge of a broken bond, part of carboxyl forms a hydration layer on the surface of the clay particles through hydration, and the potential on the surface of the clay particles is increased. And the molecular chain of the cellulose macromolecule is longer, one molecule can adsorb a plurality of clay particles at the same time to form a mixed net structure with the clay particles, so that the clay particles are prevented from being bonded with each other to be enlarged, the coalescence stability of the clay particles is greatly improved, a compact and tough filter cake is formed, the effect of reducing the filtration loss can be achieved, and the pore blocking effect of the cellulose macromolecule can reduce the filtration loss, so that the good filtration loss reducing effect is achieved finally.
According to the method, firstly, alkyl vinyl ester monomers are subjected to emulsion polymerization under the action of an emulsifier and an initiator, then, under the action of a crosslinking agent, grafting crosslinking is formed between the formed ester polymers and cellulose macromolecules, so that crosslinking between the vinyl ester monomer polymers and the cellulose macromolecules is realized, and a net structure is formed, so that the high-temperature resistance of cellulose can be improved, the obtained filtrate reducer also has excellent salt resistance, and probably, because hydroxyl groups and other groups on a cellulose molecular chain can be adsorbed on a shale interface as hydrophilic ends, and the vinyl ester polymers can cover the shale surface as lipophilic ends, the mud cake quality is improved, the filtrate loss of drilling fluid is reduced, and the moisture dispersion of shale particles is prevented. The finally obtained filtrate reducer has excellent high temperature resistance, salt resistance, calcium resistance and beauty resistance, and also has excellent filtrate reducer performance. And in addition, the raw materials adopt cellulose and alkyl esters, compared with humic acid and resin filtrate reducer, the filtrate reducer is colorless, has small influence on the surrounding environment in the drilling effect, is easier to treat after operation, reduces the treatment cost of waste slurry, is more environment-friendly, and has wide application prospect as an environment-friendly filtrate reducer.
Optionally, the alkyl vinyl acetate monomer is one or more of vinyl acrylate, vinyl acetate, methyl methacrylate and butyl methacrylate;
and/or the cellulose is one or two of carboxymethyl cellulose and hydroxyethyl cellulose.
Optionally, the alkyl vinyl acetate monomer is selected from the following monomers in a mass ratio of 1: vinyl acetate and vinyl acrylate of (1-2).
By adopting the technical scheme, the fluid loss agent finally obtained by adopting the monomers has better fluid loss and high temperature resistance.
Optionally, the raw material of the fluid loss additive further comprises 0.1-0.3 parts by weight of sodium metabisulfite.
By adopting the technical scheme, the residual monomers after the alkyl vinyl acetate monomers are polymerized can be removed by adding the sodium pyrosulfite, so that the crosslinking between the cellulose and the copolymer in the system is finally ensured, and the uniform filtrate reducer emulsion is finally obtained.
Optionally, the raw materials of the fluid loss additive also comprise 0.05-0.15 weight part of polyvinyl alcohol.
Through adopting above-mentioned technical scheme, the addition of polyvinyl alcohol probably prevents the effect in two aspects because the film forming separation hinders with the thickening and plays good fluid loss effect, can form certain sodium polyacrylate after the polymerization of alkyl acid vinyl ester monomer in this application moreover, and sodium polyacrylate can play certain viscosity reduction effect to make polyvinyl alcohol when playing the fluid loss effect to a certain extent, still can not show the construction difficulty that increases the viscosity of fluid loss agent and lead to.
Optionally, the initiator is one or two of potassium persulfate and ammonium persulfate.
By adopting the technical scheme, when the potassium persulfate and/or the ammonium persulfate are selected, the initiator effect can be achieved, potassium ions and/or ammonium ions are introduced into the system, the system is easy to be embedded into a hexagonal ring, the inhibition on clay hydration is strong, the drilling fluid filtration loss can be reduced, the salt resistance and the viscosity are not increased, the synergistic effect is good when the drilling fluid is compounded with polyvinyl alcohol, and the excellent filtration loss reduction performance can be achieved.
Optionally, the cross-linking agent is one or two of 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide and N-hydroxymethyl acrylamide;
the emulsifier is one or more of nonylphenol polyoxyethylene ether, octylphenol polyoxyethylene ether and fatty alcohol polyoxyethylene ether.
In a second aspect, the application provides a preparation method of an environment-friendly high-temperature resistant filtrate reducer, comprising the following steps:
preparing a pre-emulsion: stirring and emulsifying alkyl vinyl ester monomer, emulsifier, cross-linking agent and (1/5-2/5) water to prepare pre-emulsion;
preparing a filtrate reducer: and mixing the obtained pre-emulsion with an initiator, stirring to obtain a mixed emulsion, dripping the mixed emulsion into the residual water with the temperature of 65-80 ℃, adding cellulose, carrying out heat preservation reaction, and adjusting the pH value to be alkalescent to obtain the fluid loss additive.
By adopting the technical scheme, the vinyl alkyl acid ester monomer is firstly prepared into the pre-emulsion, then the initiator is added for emulsion polymerization, then the mixed emulsion is dripped into water, and then the cellulose is added, so that the emulsion forms liquid drops in the water, and at the moment, the cellulose and the emulsion liquid drops are subjected to cross-linking grafting on the surface to form macromolecular emulsion, thereby achieving good fluid loss reduction effect.
Optionally, in the step of preparing the fluid loss additive, the cellulose is added, then the reaction is carried out for 50-70min, then sodium metabisulfite is added, then the reaction is continued for 2-3h, and the pH is adjusted to obtain the fluid loss additive.
By adopting the technical scheme, the addition of the sodium metabisulfite can remove the residual monomers during the polymerization of the vinyl alkyl acid ester monomers, and prevent the residual monomers from polymerizing or grafting with the cellulose, so that the residual monomers are agglomerated in the emulsion, thereby ensuring that the crosslinking between the cellulose and the copolymer is finally carried out in the system, and finally obtaining the uniform filtrate reducer emulsion.
Optionally, the raw material of the fluid loss additive also comprises 0.05-0.15 weight part of polyvinyl alcohol;
in the preparation step of the fluid loss additive, the polyvinyl alcohol is added while the cellulose is added.
In summary, the present application has the following beneficial effects:
1. according to the method, firstly, alkyl acid vinyl ester monomers are subjected to emulsion polymerization under the action of an emulsifier and an initiator, and then, under the action of a cross-linking agent, graft cross-linking is formed between the formed ester polymers and cellulose macromolecules, so that cross-linking between the vinyl ester monomer polymers and the cellulose macromolecules is realized, and the prepared fluid loss additive has excellent high-temperature resistance, salt resistance, calcium resistance and aesthetic resistance and also has excellent fluid loss reduction performance;
2. compared with humic acid and resin filtrate reducers, the filtrate reducer is colorless, has little influence on the surrounding environment when used for drilling, is easier to treat after operation, reduces the treatment cost of waste slurry, is more environment-friendly, and has wide application prospect when used as an environment-friendly filtrate reducer;
3. the addition of the polyvinyl alcohol in the application can play a good fluid loss reducing effect due to the effects of film forming obstruction and thickening obstruction, a certain amount of sodium polyacrylate can be formed after polymerization of the vinyl alkanoate monomer in the application, and the sodium polyacrylate can play a certain viscosity reducing effect, so that the polyvinyl alcohol can play a fluid loss reducing effect to a certain extent, and meanwhile, the construction difficulty caused by the viscosity of the fluid loss reducer cannot be obviously increased;
4. the residual monomers during the polymerization of alkyl acid vinyl ester monomer can be got rid of in the addition of sodium metabisulfite in this application, prevents to take place polymerization or grafting between residual monomer and the cellulose to the caking in the emulsion, thereby the final cross-linking between cellulose and the copolymer in the guarantee system, finally obtain even fluid loss additive emulsion.
Detailed Description
The present application is further described in detail with reference to the following examples, which are specifically illustrated by the following: the following examples, in which specific conditions are not specified, were carried out according to conventional conditions or conditions recommended by the manufacturer, and the starting materials used in the following examples are available from ordinary commercial sources unless otherwise specified.
Sodium polyacrylate emulsions in the following examples and comparative examples were available from Henan Huashuo chemical products, inc.
Examples
Example 1
A preparation method of an environment-friendly high-temperature resistant fluid loss agent comprises the following steps:
preparing a pre-emulsion: stirring and emulsifying 50kg of alkyl vinyl acetate monomer, 5kg of emulsifier, 10kg of cross-linking agent and 10kg of water to prepare pre-emulsion;
preparing a filtrate reducer: and mixing the obtained pre-emulsion with 1kg of initiator, stirring to obtain a mixed emulsion, then dropwise adding the mixed emulsion into 20kg of 70 ℃ water, then adding 10kg of carboxymethyl cellulose, carrying out heat preservation reaction for 3 hours, and adding sodium hydroxide to adjust the pH value to 8 to obtain the fluid loss additive.
Wherein, the alkyl vinyl acetate monomer comprises vinyl acetate and vinyl acrylate with the mass ratio of 1.5, the emulsifier adopts nonylphenol polyoxyethylene ether NP-10, the cross-linking agent adopts 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide, and the initiator adopts potassium persulfate.
Example 2
A preparation method of an environment-friendly high-temperature resistant fluid loss agent comprises the following steps:
preparing a pre-emulsion: stirring and emulsifying 40kg of alkyl vinyl acetate monomer, 3kg of emulsifier, 7kg of cross-linking agent and 8kg of water to prepare pre-emulsion;
preparing a filtrate reducer: and mixing the obtained pre-emulsion with 0.5kg of initiator, stirring to obtain mixed emulsion, dripping the mixed emulsion into 12kg of 65 ℃ water, adding 8kg of carboxymethyl cellulose, carrying out heat preservation reaction for 2 hours, adding sodium hydroxide, and adjusting the pH value to 7 to obtain the fluid loss additive.
Wherein, the alkyl vinyl acetate monomer comprises vinyl acetate and methyl methacrylate with the mass ratio of 1.
Example 3
A preparation method of an environment-friendly high-temperature resistant fluid loss agent comprises the following steps:
preparing a pre-emulsion: stirring and emulsifying 60kg of alkyl vinyl ester monomer, 8kg of emulsifier, 15kg of cross-linking agent and 15kg of water to prepare pre-emulsion;
preparing a filtrate reducer: and mixing the obtained pre-emulsion with 1.5kg of initiator, stirring to obtain mixed emulsion, dripping the mixed emulsion into 30kg of water with the temperature of 80 ℃, adding 15kg of hydroxyethyl cellulose, carrying out heat preservation reaction for 4 hours, adding sodium hydroxide, and adjusting the pH value to 9 to obtain the fluid loss additive.
Wherein, the alkyl vinyl acetate monomer comprises butyl methacrylate and vinyl acrylate with the mass ratio of 1.
Example 4
The preparation method of the environment-friendly high-temperature-resistant filtrate reducer is carried out according to the method in the embodiment 1, and is characterized in that in the preparation step of the filtrate reducer, cellulose is added for heat preservation reaction for 1 hour, then 0.2kg of sodium metabisulfite is added, then the heat preservation reaction is continued for 2 hours, and then the pH is adjusted.
Example 5
The preparation method of the environment-friendly high-temperature-resistant fluid loss agent is carried out according to the method in the embodiment 1, and is characterized in that in the fluid loss agent preparation step, cellulose is added and subjected to heat preservation reaction for 50min, then 0.1kg of sodium metabisulfite is added, and after the heat preservation reaction is continued for 2h, the pH value is adjusted.
Example 6
The preparation method of the environment-friendly high-temperature-resistant filtrate reducer is carried out according to the method in the embodiment 1, and is characterized in that in the filtrate reducer preparation step, cellulose is added for heat preservation reaction for 70min, then 0.3kg of sodium metabisulfite is added, then the heat preservation reaction is continued for 3h, and then the pH is adjusted.
Example 7
The preparation method of the environment-friendly high-temperature-resistant fluid loss additive is carried out according to the method in the embodiment 4, and is characterized in that in the preparation step of the fluid loss additive, 0.1kg of polyvinyl alcohol is added while cellulose is added.
Example 8
The preparation method of the environment-friendly high-temperature-resistant fluid loss additive is carried out according to the method in the embodiment 4, and is characterized in that in the preparation step of the fluid loss additive, 0.05kg of polyvinyl alcohol is added while cellulose is added.
Example 9
The preparation method of the environment-friendly high-temperature-resistant fluid loss additive is carried out according to the method in the embodiment 4, and is characterized in that in the preparation step of the fluid loss additive, 0.15kg of polyvinyl alcohol is added while cellulose is added.
Example 10
The preparation method of the environment-friendly high-temperature resistant fluid loss additive is carried out according to the method in the embodiment 4, and is characterized in that vinyl acrylate and methyl methacrylate with the mass ratio of 1.
Example 11
The preparation method of the environment-friendly high-temperature-resistant fluid loss additive is carried out according to the method in the embodiment 4, and the difference is that dimethyl azodiisobutyrate is used as the initiator.
Comparative example
Comparative example 1
A method for preparing a fluid loss additive, carried out according to the method in example 1, except that cellulose and a cross-linking agent are not added to the raw materials.
Comparative example 2
A method for producing a fluid loss additive according to the method in example 1, except that cellulose is not added to the raw material.
Comparative example 3
A fluid loss additive was prepared as in example 1, except that vinyl acetate was replaced with acrylic acid in equal amounts.
Comparative example 4
A method for preparing a fluid loss additive, which comprises the following steps of example 1, except that the mixed emulsion is replaced by sodium polyacrylate emulsion in equal amount.
Comparative example 5
A method for the preparation of a fluid loss additive according to example 1, except that the amount of the crosslinking agent added was 6kg.
Comparative example 6
A method for the preparation of a fluid loss additive, carried out as in example 1, except that the amount of cross-linking agent added was 16kg.
Comparative example 7
A method for producing a fluid loss additive, according to the method in example 4, except that polyvinyl alcohol was replaced with cellulose in equal amounts.
Performance detection
1. Appearance inspection
The preparation of the fluid loss additive was carried out according to the methods of the above examples and comparative examples, and then the appearance of the fluid loss additive was examined, and the fluid loss additive prepared in this application was in the form of a homogeneous, light milky emulsion, which did not have a significant effect on the surrounding environment and was easier to handle when applied to drilling operations, especially in seawater operations.
2. Other Performance detection
a. Apparent viscosity measurement of 1% aqueous solution
400ml of tap water was measured, 4g of the sample was added thereto under high-speed stirring, and after stirring for 5 minutes, phi 600 reading was measured with a six-speed viscometer and the apparent viscosity was calculated.
b. 170 ℃ high-temperature high-pressure filtration loss reduction rate detection
(1) Preparing base slurry: according to the weight percentage of distilled water: sodium bentonite for preparing slurry in test: anhydrous sodium carbonate =400: preparing base slurry according to the proportion of 20;
(2) And (3) base slurry performance determination: taking 400mL of the base slurry prepared in the step (1), stirring at a high speed for 5min, then measuring the filtration loss of the base slurry, wherein the measurement result is within the range of 50 +/-10 mL, otherwise, adjusting the addition amount of the sodium bentonite for the test slurry preparation for the test;
(3) 400ml of the base slurry adjusted in (2) was taken out, and 12.0 g of the samples of the fluid loss additives obtained in examples and comparative examples were added with stirring, stirred at a high speed for 20 minutes, at least twice during which, to scrape off the sample piece adhering to the wall of the vessel, and the rate of decrease in fluid loss at 170 ℃ and 3450KPa was measured.
The reduction rate = (A-B)/A x 100%, wherein A is the high-temperature high-pressure filtration loss of the base slurry, and B is the high-temperature high-pressure filtration loss after sample addition. The results are shown in table 1 below.
c. 10% NaCl API assay
(1) Preparation of base slurry
According to the weight percentage of distilled water: sodium chloride: sodium bentonite for preparing slurry in test: preparing base slurry according to the proportion of anhydrous sodium carbonate = 400;
(2) Determination of base stock Properties
Taking 400ml of the base slurry prepared in the step (1), stirring at a high speed for 5min, measuring the filtration loss of the base slurry, wherein the measurement result is within the range of 120 +/-10 ml, and otherwise, adjusting the addition amount of the sodium bentonite for the test slurry preparation for the test;
(3) 170 ℃ Performance measurement of test slurries
Taking 400ml of the base slurry adjusted in the step (2), adding 16.0 g of the sample of the fluid loss additive prepared in the example and the comparative example under stirring, stirring at a high speed for 20min, stopping at least twice during stirring, scraping off a sample piece adhered to the wall of a container, transferring the sample piece into an aging tank, aging at 170 ℃ for 16h, taking out, and measuring the API value at room temperature. The measurement results are shown in table 1 below.
Table 1:
| detecting items | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Example 7 | Example 8 | Example 9 |
| Filtration loss reduction at 170 ℃/% | 54.8 | 52.3 | 53.1 | 62.4 | 60.2 | 61.3 | 66.8 | 65.4 | 66.1 |
| 10% NaCl API (aged 16h at 180 ℃ C.)/ml | 22.7 | 23.8 | 24.1 | 20.9 | 21.3 | 22.1 | 19.8 | 20.2 | 20.6 |
| Apparent viscosity/Mpa.s of 1% aqueous solution | 58.7 | 59.3 | 67.9 | 64.2 | 62.8 | 61.7 | 66.9 | 67.1 | 67.5 |
| Detecting items | Example 10 | Example 11 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | Comparative example 6 | Comparative example 7 |
| Filtration loss reduction at 170 ℃/% | 54.8 | 56.4 | 41.9 | 42.5 | 45.8 | 49.7 | 50.6 | 53.9 | 55.2 |
| 10% NaCl API (aged 16h at 180 ℃ C.)/ml | 24.3 | 24.8 | 28.6 | 27.1 | 26.3 | 25.6 | 25.1 | 24.8 | 22.9 |
| Apparent viscosity/Mpa.s of 1% aqueous solution | 63.8 | 61.4 | 42.8 | 43.7 | 48.2 | 46.8 | 56.1 | 59.8 | 61.8 |
As can be seen from the above table 1, the fluid loss additive prepared by the method has excellent high-temperature fluid loss performance and salt resistance, and the apparent viscosity of the fluid loss additive is 55-70Mpa.s, so that the fluid loss additive can play a good fluid loss reducing effect and cannot increase the construction difficulty due to excessive viscosity.
Referring to the detection results of the embodiment 1 and the embodiments 4 to 6, it can be seen that the addition of sodium metabisulfite can significantly increase the fluid loss performance of the fluid loss additive, and in combination with the detection results of the embodiments 7 to 9, it can be seen that the addition of polyvinyl alcohol can further enhance the fluid loss performance of the fluid loss additive; it can also be seen that the addition of polyvinyl alcohol significantly enhances fluid loss performance while having a small change in viscosity. Referring to the test results of example 10, it can be seen that the vinyl acrylate and vinyl acetate are better used as the alkyl vinyl acetate monomer; in combination with the detection results of example 11, it can be seen that the fluid loss reducing effect is better when the initiator is potassium persulfate or ammonium persulfate compared with that of the azo initiator;
referring to the test results of example 1 and comparative examples 1 and 2, it can be seen that the fluid loss reducing effect of the fluid loss additive is poor when no cellulose and cross-linking agent are added to the raw material, and the fluid loss reducing effect is slightly improved when only the cross-linking agent is added and no cellulose is added, and only cross-linking between polymers is possible, but the fluid loss reducing effect is still poor; referring to the detection result of comparative example 3, it can be seen that when the ester monomer and acrylic acid are selected as monomers, the fluid loss reduction effect is increased, but still poor; the detection result in the comparative example 4 is combined, so that the acrylic acid polymer and the cellulose are directly crosslinked, and the fluid loss effect of the fluid loss additive is still poor, and the detection results of the comparative examples 5 and 6 are referred, so that the fluid loss effect is poor when the addition amount of the crosslinking agent is too low, and the fluid loss effect is slightly changed or even slightly reduced when the addition amount of the crosslinking agent is too large; referring to the test results of comparative example 7, it can be seen that when the amount of cellulose added is increased, the fluid loss effect change is smaller, which is much lower than the performance of the fluid loss additive obtained by adding cellulose and polyvinyl alcohol after polymerization.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (5)
1. The environment-friendly high-temperature-resistant fluid loss agent is characterized by being prepared from the following raw materials in parts by weight:
40-60 parts of a mixture with the mass ratio of 1: (1-2) vinyl acetate and vinyl acrylate, 3-8 parts of an emulsifier, 7-15 parts of a crosslinking agent, 0.5-1.5 parts of an initiator, 8-15 parts of cellulose and 20-45 parts of water;
the raw material of the filtrate reducer also comprises 0.1-0.3 weight part of sodium metabisulfite;
the cellulose is one or two of carboxymethyl cellulose and hydroxyethyl cellulose;
the cross-linking agent is one or two of 2, 5-dimethyl-2, 5-di-tert-butyl hexane peroxide and N-hydroxymethyl acrylamide;
the emulsifier is one or more of nonylphenol polyoxyethylene ether, octylphenol polyoxyethylene ether and fatty alcohol polyoxyethylene ether;
the preparation method of the high-temperature resistant fluid loss agent comprises the following steps:
preparing a pre-emulsion: stirring and emulsifying vinyl acetate, vinyl acrylate, an emulsifier, a cross-linking agent and 1/5-2/5 of water to prepare a pre-emulsion;
preparing a filtrate reducer: and mixing the obtained pre-emulsion with an initiator, stirring to obtain a mixed emulsion, dripping the mixed emulsion into the residual water with the temperature of 65-80 ℃, adding cellulose, reacting, and adjusting the pH value to be alkalescent to obtain the fluid loss additive.
2. The environment-friendly high-temperature-resistant fluid loss additive as defined in claim 1, wherein: the raw materials of the fluid loss additive also comprise 0.05-0.15 weight part of polyvinyl alcohol.
3. The environment-friendly high-temperature-resistant fluid loss additive as defined in claim 1, wherein: the initiator is one or two of potassium persulfate and ammonium persulfate.
4. The preparation method of the environment-friendly high-temperature-resistant fluid loss additive as defined in claim 1, wherein the preparation method comprises the following steps: the method comprises the following steps:
preparing a pre-emulsion: stirring and emulsifying vinyl acetate, vinyl acrylate, an emulsifier, a cross-linking agent and 1/5-2/5 of water to prepare a pre-emulsion;
preparing a filtrate reducer: mixing the obtained pre-emulsion with an initiator, stirring to obtain a mixed emulsion, then dropwise adding the mixed emulsion into the residual water at 65-80 ℃, adding cellulose, reacting, and adjusting the pH value to alkalescence to obtain a filtrate reducer;
in the preparation step of the filtrate reducer, the cellulose is added, the reaction is carried out for 50-70min, then the sodium metabisulfite is added, the reaction is continued for 2-3h, and the pH is adjusted to obtain the filtrate reducer.
5. The preparation method of the environment-friendly high temperature resistant fluid loss additive according to claim 4, wherein the preparation method comprises the following steps: the raw materials of the fluid loss additive also comprise 0.05 to 0.15 weight part of polyvinyl alcohol;
in the preparation step of the fluid loss additive, the polyvinyl alcohol is added while the cellulose is added.
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