CN114805705A - High-temperature-resistant filtrate loss reducer sodium humate for well drilling and preparation method thereof - Google Patents
High-temperature-resistant filtrate loss reducer sodium humate for well drilling and preparation method thereof Download PDFInfo
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- 239000011734 sodium Substances 0.000 title claims abstract description 61
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 title claims abstract description 59
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 59
- 238000005553 drilling Methods 0.000 title claims abstract description 35
- 239000000706 filtrate Substances 0.000 title claims abstract description 35
- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000003245 coal Substances 0.000 claims abstract description 113
- 238000006243 chemical reaction Methods 0.000 claims abstract description 82
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 78
- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 claims abstract description 73
- 239000004021 humic acid Substances 0.000 claims abstract description 73
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 56
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 50
- GQOKIYDTHHZSCJ-UHFFFAOYSA-M dimethyl-bis(prop-2-enyl)azanium;chloride Chemical compound [Cl-].C=CC[N+](C)(C)CC=C GQOKIYDTHHZSCJ-UHFFFAOYSA-M 0.000 claims abstract description 26
- 239000011787 zinc oxide Substances 0.000 claims abstract description 25
- UOULCEYHQNCFFH-UHFFFAOYSA-M sodium;hydroxymethanesulfonate Chemical compound [Na+].OCS([O-])(=O)=O UOULCEYHQNCFFH-UHFFFAOYSA-M 0.000 claims abstract description 20
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 230000007062 hydrolysis Effects 0.000 claims abstract description 11
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 11
- 230000003647 oxidation Effects 0.000 claims abstract description 11
- 230000003197 catalytic effect Effects 0.000 claims abstract description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 35
- 238000004132 cross linking Methods 0.000 claims description 25
- 239000000654 additive Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 12
- 230000000996 additive effect Effects 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 6
- 238000000605 extraction Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000007800 oxidant agent Substances 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 238000005086 pumping Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 239000002699 waste material Substances 0.000 abstract description 4
- 239000002002 slurry Substances 0.000 description 9
- 239000012530 fluid Substances 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 239000002585 base Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- -1 aliphatic aromatic hydroxycarboxylic acids Chemical class 0.000 description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 238000005189 flocculation Methods 0.000 description 3
- 230000016615 flocculation Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- SIKJAQJRHWYJAI-UHFFFAOYSA-N Indole Chemical compound C1=CC=C2NC=CC2=C1 SIKJAQJRHWYJAI-UHFFFAOYSA-N 0.000 description 2
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000008186 active pharmaceutical agent Substances 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000006277 sulfonation reaction Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229920001732 Lignosulfonate Polymers 0.000 description 1
- 229930192627 Naphthoquinone Natural products 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 230000009920 chelation Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- UPHIPHFJVNKLMR-UHFFFAOYSA-N chromium iron Chemical compound [Cr].[Fe] UPHIPHFJVNKLMR-UHFFFAOYSA-N 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- SOCTUWSJJQCPFX-UHFFFAOYSA-N dichromate(2-) Chemical compound [O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O SOCTUWSJJQCPFX-UHFFFAOYSA-N 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- PZOUSPYUWWUPPK-UHFFFAOYSA-N indole Natural products CC1=CC=CC2=C1C=CN2 PZOUSPYUWWUPPK-UHFFFAOYSA-N 0.000 description 1
- RKJUIXBNRJVNHR-UHFFFAOYSA-N indolenine Natural products C1=CC=C2CC=NC2=C1 RKJUIXBNRJVNHR-UHFFFAOYSA-N 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011499 joint compound Substances 0.000 description 1
- 150000002605 large molecules Chemical class 0.000 description 1
- 239000003077 lignite Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 150000002791 naphthoquinones Chemical class 0.000 description 1
- 238000010525 oxidative degradation reaction Methods 0.000 description 1
- 239000003415 peat Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 125000004151 quinonyl group Chemical group 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F289/00—Macromolecular compounds obtained by polymerising monomers on to macromolecular compounds not provided for in groups C08F251/00 - C08F287/00
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- 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
Abstract
The invention belongs to a high temperature resistant filtrate loss reducer sodium humate for well drilling and a preparation method thereof; the sodium humate filtrate reducer is prepared from the following raw materials: weathered coal with low humic acid content, sodium hydroxymethyl sulfonate, sodium hydroxide, nano zinc oxide, dimethyl diallyl ammonium chloride and water; the weathered coal with low humic acid content is weathered coal with 40-50% of humic acid content; the method has the advantages that the humic acid content of the weathered coal with low humic acid content is improved through hydrothermal oxidation, so that the weathered coal with low humic acid content is recycled, resource waste is avoided, and meanwhile, the basis is laid for sulfomethylation reaction through hydrolysis of humic acid of the weathered coal through high-temperature catalytic hydrolysis.
Description
Technical Field
The invention belongs to the technical field of humic acid application, and particularly relates to a high-temperature-resistant filtrate loss reducer sodium humate for well drilling and a preparation method thereof.
Background
Humic acid is a high molecular organic substance formed by animal and plant residues through a series of processes of microbial decomposition, synthesis and geochemistry, is a mixture of aliphatic aromatic hydroxycarboxylic acids with different molecular weights, and is mainly derived from weathered coal, lignite and peat. The molecular weight of the humic acid is 300-100000, the structure of the humic acid is complex, and the humic acid is generally considered to be mainly composed of a core, a bridge bond and an active group. The nucleus consists of five-membered and six-membered rings of homocyclic or heterocyclic rings, e.g. benzene ring, naphthoquinone, pyrrole, bark, indole, etc., and the bridge has two kinds of single and double bridges, e.g. -CH 2 -、＝CH-、-O-、-NH-、-CH 2 -CH 2 And the active groups are mainly more than ten of carboxyl, phenolic hydroxyl, quinonyl, alcoholic hydroxyl, sulfonic group, amino, carbonyl, methoxy and free radical, and the groups play a great role in humic acid substances used in drilling mud.
H on the acid group of humic acid + Can be covered by Na + 、K + The monovalent alkali metal ions are replaced to generate soluble humate, and the generated humate can be used as a mud treating agent for well drilling, and sodium humate, potassium humate and the like are widely used at present. In addition, the groups of-COOH and-OH in humic acid can have complexation or chelation reaction with metal ions, and the like, and simultaneously, the humic acid is differentUnder the condition, the humic acid has two properties of oxidation and reduction, and besides, the humic acid can also be hydrolyzed, sulfonated and oxidatively degraded, so that the humic acid can react with various inorganic reagents to generate various derivatives. In addition, it can be condensed with some organic matters to form some complexes, and most of the products can be used for drilling as mud treatment agents. Therefore, the application of humic acid as a drilling fluid treating agent is the most important aspect of the application of the humic acid industry and is also an important component of the petroleum drilling fluid treating agent.
Sodium humate is mainly used as a filtrate reducer and a viscosity reducer in drilling fluid, but the sodium humate is 'inherent insufficient' in high temperature resistance stability and salt resistance, and dichromate is added on the basis of HA-Na or is compounded with iron chromium lignosulfonate (FCLS) for use in order to improve the high temperature resistance of the sodium humate, and the products with chromium pollution are eliminated.
With the development of the oil and gas industry, the exploitation depth gradually increases, and the drilling and exploitation difficulty caused by high temperature and complex stratum also becomes larger and larger. Generally, the bottom temperature of a 4000m deep well can reach 150-180 ℃, and the temperature of a 7000-8000 m ultra-deep well can reach 200-250 ℃. Thus, the physicochemical changes which are not easy to occur at low temperatures are activated and displayed at high temperatures, and formation contamination (salt, calcium, mud, acid gas, etc.) is also increased, which inevitably damages or even completely destroys the original properties of the drilling fluid. The sodium humate cannot meet the requirements of drilling deep wells and complex stratums due to the defects of the structure and the performance of the sodium humate (such as poor-COOH dissociation performance and poor electrolyte flocculation resistance). This puts higher demands on the temperature and salt resistance of sodium humate as filtrate reducer.
Weathered coal is used as a raw material of humic acid sources, the price is low, the storage capacity is large, the weathered coal resources with high humic acid content and humic acid content of more than 60% are less and less along with the exploitation, but the weathered coal with the humic acid content of 40% -50% has large storage capacity, but the humic acid content of sodium humate produced by the weathered coal is low and the yield is low due to the low humic acid content, so most of the weathered coal with low humic acid content is used as waste or mixed in coal to be sent to a power plant for burning, and the part of humic acid raw material is wasted. Further, it is known from the common general knowledge in the art that weathered coal is used as mineral humic acid, and sulfonation or sulfomethylation is difficult to perform due to a large molecule, so that the hydrophilicity and electrolyte flocculation resistance of sodium humate produced by using weathered coal as a raw material cannot be improved on the premise that sulfonation or sulfomethylation reaction cannot be performed, that is, the high temperature resistance of the sodium humate filtrate reducer cannot be realized.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the high-temperature-resistant filtrate reducer sodium humate for drilling and the preparation method thereof, wherein the low-content weathered coal is used as a raw material for production, so that the low-humic acid-content weathered coal is recycled, the resource waste is avoided, the humic acid content of the low-humic acid-content weathered coal is improved through hydrothermal oxidation, and the high-temperature catalytic hydrolysis is carried out on the humic acid of the weathered coal to lay a foundation for sulfomethylation reaction.
The purpose of the invention is realized as follows:
a high-temperature resistant filtrate reducer sodium humate for well drilling is prepared from the following raw materials: weathered coal with low humic acid content, sodium hydroxymethyl sulfonate, sodium hydroxide, nano zinc oxide, dimethyl diallyl ammonium chloride and water; the weathered coal with low humic acid content is weathered coal with 40-50% of humic acid content.
The invention also provides a preparation method of the high-temperature-resistant filtrate reducer sodium humate for drilling, which comprises the following steps:
step 1: dividing water into two parts, namely a first part of water and a second part of water;
step 2: crushing weathered coal with low humic acid content, mixing the crushed weathered coal with first part of water, feeding the mixture into a hydrothermal oxidation reactor, and carrying out hydrothermal oxidation reaction to obtain oxidized weathered coal;
and step 3: putting the oxidized weathered coal and the second part of water in the step 2 into a reaction kettle, uniformly stirring, adding sodium hydroxide and nano zinc oxide, and performing catalytic hydrolysis and extraction reaction to prepare a sodium humate solution;
and 4, step 4: adding sodium hydroxymethyl sulfonate into the sodium humate solution obtained in the step 3 to perform sulfomethylation reaction;
and 5: and (3) adding dimethyldiallylammonium chloride into the solution subjected to sulfomethylation reaction in the step (4) for crosslinking reaction, pumping the material subjected to crosslinking reaction into a settling tank for settling, concentrating, drying and crushing the settled solution to be less than 0.5 mm.
Preferably, the weathered coal powder with low humic acid content in the step 2 is crushed to 40-60 meshes, and the mass ratio of the weathered coal with low humic acid content to the first part of water is as follows: 1: 3.
preferably, the reaction temperature of the hydrothermal oxidizer in the step 2 is 200 ℃, the pressure is 1.8MPa, and the mixed materials are reacted for 30 minutes under the above conditions.
Preferably, the mass ratio of the oxidized weathered coal to the second part of water in the step 3 is 1: 6; the mass ratio of the oxidized weathered coal to the sodium hydroxide is 1: 0.1-0.2; the mass ratio of the weathered coal oxide to the nano zinc oxide is 1: 0.001-0.003; the temperature of the reaction kettle after the sodium hydroxide and the nano zinc oxide are added is as follows: and reacting for 30-40 minutes at 130 ℃ under the condition of continuously stirring at 120 revolutions per minute.
Preferably, the mass ratio of the addition amount of the sodium hydroxymethyl sulfonate to the oxidized weathered coal in the step 4 is as follows: 0.05-0.2: 1;
the sulfomethylation reaction is carried out at the temperature of: continuously stirring and reacting for 2 hours at the temperature of 160-180 ℃; the stirring rate was 120 rpm.
Preferably, the mass ratio of the addition amount of the dimethyl diallyl ammonium chloride to the oxidized weathered coal in the step 5 is as follows: 0.1-0.15: 1;
before adding dimethyl diallyl ammonium chloride for crosslinking reaction, firstly cooling the solution subjected to sulfomethylation reaction to 60-80 ℃; and reacting for 20-30 minutes at a stirring speed of 120 revolutions per minute during the crosslinking reaction.
Preferably, the concentration in the step 5 is carried out at the temperature of 70-80 ℃ until the solid content is 18-22%; and the drying is carried out at the temperature of 85-90 ℃ until the water content is lower than 12%.
According to the technical scheme, the high-temperature-resistant filtrate reducer sodium humate for drilling and the preparation method thereof are prepared, weathered coal with the humic acid content of 40-50% is selected, so that the weathered coal with the low humic acid content can be recycled, and the manufacturing cost of the sodium humate filtrate reducer can be reduced; meanwhile, the weathered coal is subjected to oxidative degradation through hydrothermal oxidation, the humic acid content of the weathered coal is improved, and the weathered coal and sodium hydroxymethyl sulfonate are easy to generate sulfomethylation reaction through catalytic hydrolysis, so that sodium humate prepared from the weathered coal is subjected to sulfomethylation modification, the hydrophilicity and the electrolyte flocculation resistance are increased, the characteristic of increasing the high-temperature resistance of the sodium humate is realized by selecting dimethyl diallyl ammonium chloride for crosslinking reaction, and the defect that formaldehyde, phenol and the like have pollutants on the environment is avoided; the method has the advantages that the low-content weathered coal is used as a raw material for production, the low-humic-acid-content weathered coal is recycled, resource waste is avoided, the humic acid content of the low-humic-acid-content weathered coal is improved through hydrothermal oxidation, and a foundation is laid for sulfomethylation reaction of humic acid of the weathered coal through high-temperature catalytic hydrolysis.
Detailed Description
The invention relates to a high-temperature resistant filtrate reducer sodium humate for well drilling and a preparation method thereof, wherein the sodium humate filtrate reducer is prepared from the following raw materials: weathered coal with low humic acid content, sodium hydroxymethyl sulfonate, sodium hydroxide, nano zinc oxide, dimethyl diallyl ammonium chloride and water; the weathered coal with low humic acid content is weathered coal with 40-50% of humic acid content.
The invention also provides a preparation method of the high-temperature-resistant filtrate reducer sodium humate for drilling, which comprises the following steps:
step 1: dividing water into two parts, namely a first part of water and a second part of water;
step 2: crushing weathered coal with low humic acid content, mixing the crushed weathered coal with first part of water, feeding the mixture into a hydrothermal oxidation reactor, and carrying out hydrothermal oxidation reaction to obtain oxidized weathered coal;
and step 3: putting the oxidized weathered coal and the second part of water in the step 2 into a reaction kettle, uniformly stirring, adding sodium hydroxide and nano zinc oxide, and performing catalytic hydrolysis and extraction reaction to prepare a sodium humate solution;
and 4, step 4: adding sodium hydroxymethyl sulfonate into the sodium humate solution obtained in the step 3 to perform sulfomethylation reaction;
and 5: and (3) adding dimethyldiallylammonium chloride into the solution subjected to sulfomethylation reaction in the step (4) for crosslinking reaction, pumping the material subjected to crosslinking reaction into a settling tank for settling, concentrating, drying and crushing the settled solution to be less than 0.5 mm.
Further, the weathered coal powder with low humic acid content in the step 2 is crushed to 40-60 meshes, and the mass ratio of the weathered coal with low humic acid content to the first part of water is as follows: 1: 3.
further, the reaction temperature of the hydrothermal oxidizer in the step 2 is 200 ℃, the pressure is 1.8MPa, and the mixed material is reacted for 30 minutes under the above conditions.
Further, the mass ratio of the oxidized weathered coal to the second part of water in the step 3 is 1: 6; the mass ratio of the oxidized weathered coal to the sodium hydroxide is 1: 0.1-0.2; the mass ratio of the oxidized weathered coal to the nano zinc oxide is 1: 0.001-0.003; the temperature of the reaction kettle after the sodium hydroxide and the nano zinc oxide are added is as follows: and reacting for 30-40 minutes at 130 ℃ under the condition of continuously stirring at 120 revolutions per minute.
Further, the mass ratio of the addition amount of the sodium hydroxymethyl sulfonate to the oxidized weathered coal in the step 4 is as follows: 0.05-0.2: 1;
the sulfomethylation reaction is carried out at the temperature of: continuously stirring and reacting for 2 hours at the temperature of 160-180 ℃; the stirring rate was 120 rpm.
Further, the mass ratio of the addition amount of the dimethyl diallyl ammonium chloride to the oxidized weathered coal in the step 5 is as follows: 0.1-0.15: 1;
before adding dimethyl diallyl ammonium chloride for crosslinking reaction, firstly cooling the solution subjected to sulfomethylation reaction to 60-80 ℃; and reacting for 20-30 minutes at a stirring speed of 120 revolutions per minute during the crosslinking reaction.
Further, the concentration in the step 5 is carried out at the temperature of 70-80 ℃ until the solid content is 18-22%; and the drying is carried out at the temperature of 85-90 ℃ until the water content is lower than 12%.
In order to explain the present invention more clearly, the present invention will now be further described with reference to specific examples. Specific examples are as follows:
example one
The high-temperature resistant filtrate reducer sodium humate for drilling comprises the following raw materials: weathered coal with low humic acid content, sodium hydroxymethyl sulfonate, sodium hydroxide, nano zinc oxide, dimethyl diallyl ammonium chloride and water; the weathered coal with low humic acid content is weathered coal with 40-50% of humic acid content.
A preparation method of a high-temperature resistant filtrate reducer sodium humate for drilling comprises the following steps:
step 1: dividing water into two parts, namely a first part of water and a second part of water;
step 2: crushing weathered coal with low humic acid content, mixing the crushed weathered coal with first part of water, feeding the mixture into a hydrothermal oxidation reactor, and carrying out hydrothermal oxidation reaction to obtain oxidized weathered coal;
and step 3: putting the oxidized weathered coal and the second part of water in the step 2 into a reaction kettle, uniformly stirring, adding sodium hydroxide and nano zinc oxide, and performing catalytic hydrolysis and extraction reaction to prepare a sodium humate solution;
and 4, step 4: adding sodium hydroxymethyl sulfonate into the sodium humate solution obtained in the step 3 to perform sulfomethylation reaction;
and 5: and (3) adding dimethyldiallylammonium chloride into the solution subjected to sulfomethylation reaction in the step (4) for crosslinking reaction, pumping the material subjected to crosslinking reaction into a settling tank for settling, concentrating, drying and crushing the settled solution to be less than 0.5 mm.
The weathered coal powder with low humic acid content in the step 2 is crushed to 40-60 meshes, and the mass ratio of the weathered coal with low humic acid content to the first part of water is as follows: 1: 3. the reaction temperature of the hydrothermal oxidizer in the step 2 is 200 ℃, the pressure is 1.8MPa, and the mixed materials are reacted for 30 minutes under the conditions. The mass ratio of the oxidized weathered coal to the second part of water in the step 3 is 1: 6; the mass ratio of the oxidized weathered coal to the sodium hydroxide is 1: 0.1; the mass ratio of the oxidized weathered coal to the nano zinc oxide is 1: 0.001; the temperature of the reaction kettle after the sodium hydroxide and the nano zinc oxide are added is as follows: the reaction was carried out at 130 ℃ for 30 minutes with continuous stirring at 120 rpm. The mass ratio of the addition amount of the sodium hydroxymethyl sulfonate to the oxidized weathered coal in the step 4 is as follows: 0.05: 1; the sulfomethylation reaction is carried out at the temperature of: continuously stirring and reacting for 2 hours at the temperature of 160 ℃; the stirring rate was 120 rpm. The mass ratio of the addition amount of the dimethyl diallyl ammonium chloride to the oxidized weathered coal in the step 5 is as follows: 0.1-0.15: 1; before adding dimethyl diallyl ammonium chloride for crosslinking reaction, firstly cooling the solution subjected to sulfomethylation reaction to 60-80 ℃; and reacting for 20-30 minutes at a stirring speed of 120 revolutions per minute during the crosslinking reaction. The concentration in the step 5 is carried out at the temperature of 70-80 ℃ until the solid content is 18-22%; the drying is carried out at 85-90 ℃ until the water content is 11%.
Example two
The high-temperature resistant filtrate reducer sodium humate for drilling comprises the following raw materials: weathered coal with low humic acid content, sodium hydroxymethyl sulfonate, sodium hydroxide, nano zinc oxide, dimethyl diallyl ammonium chloride and water; the weathered coal with low humic acid content is weathered coal with 40-50% of humic acid content.
A preparation method of a high-temperature resistant filtrate reducer sodium humate for drilling comprises the following steps:
step 1: dividing water into two parts, namely a first part of water and a second part of water;
step 2: crushing weathered coal with low humic acid content, mixing the crushed weathered coal with first part of water, feeding the mixture into a hydrothermal oxidation reactor, and carrying out hydrothermal oxidation reaction to obtain oxidized weathered coal;
and step 3: putting the oxidized weathered coal and the second part of water in the step 2 into a reaction kettle, uniformly stirring, adding sodium hydroxide and nano zinc oxide, and performing catalytic hydrolysis and extraction reaction to prepare a sodium humate solution;
and 4, step 4: adding sodium hydroxymethyl sulfonate into the sodium humate solution obtained in the step 3 to perform sulfomethylation reaction;
and 5: and (3) adding dimethyldiallylammonium chloride into the solution subjected to sulfomethylation reaction in the step (4) for crosslinking reaction, pumping the material subjected to crosslinking reaction into a settling tank for settling, concentrating, drying and crushing the settled solution to be less than 0.5 mm.
The weathered coal powder with low humic acid content in the step 2 is crushed to 40-60 meshes, and the mass ratio of the weathered coal with low humic acid content to the first part of water is as follows: 1: 3. the reaction temperature of the hydrothermal oxidizer in the step 2 is 200 ℃, the pressure is 1.8MPa, and the mixed materials are reacted for 30 minutes under the conditions. The mass ratio of the oxidized weathered coal to the second part of water in the step 3 is 1: 6; the mass ratio of the oxidized weathered coal to the sodium hydroxide is 1: 0.2; the mass ratio of the oxidized weathered coal to the nano zinc oxide is 1: 0.003; the temperature of the reaction kettle after the sodium hydroxide and the nano zinc oxide are added is as follows: the reaction was carried out at 130 ℃ for 40 minutes with continuous stirring at 120 rpm. The mass ratio of the addition amount of the sodium hydroxymethyl sulfonate to the oxidized weathered coal in the step 4 is as follows: 0.2: 1; the sulfomethylation reaction is carried out at the temperature of: continuously stirring and reacting for 2 hours at the temperature of 180 ℃; the stirring rate was 120 rpm. The mass ratio of the addition amount of the dimethyl diallyl ammonium chloride to the oxidized weathered coal in the step 5 is as follows: 0.15: 1; before adding dimethyl diallyl ammonium chloride for crosslinking reaction, firstly cooling the solution subjected to sulfomethylation reaction to 80 ℃; the crosslinking reaction was carried out for 30 minutes at a stirring rate of 120 rpm. The concentration in the step 5 is to concentrate the mixture to a solid content of 22% in an environment with a temperature of 80 ℃; the drying is carried out at 85-90 ℃ until the water content is 10%.
EXAMPLE III
The high-temperature resistant filtrate reducer sodium humate for drilling comprises the following raw materials: weathered coal with low humic acid content, sodium hydroxymethyl sulfonate, sodium hydroxide, nano zinc oxide, dimethyl diallyl ammonium chloride and water; the weathered coal with low humic acid content is weathered coal with 40-50% of humic acid content.
A preparation method of a high-temperature resistant filtrate reducer sodium humate for drilling comprises the following steps:
step 1: dividing water into two parts, namely a first part of water and a second part of water;
and 2, step: crushing weathered coal with low humic acid content, mixing the crushed weathered coal with first part of water, and then feeding the mixture into a hydrothermal oxidation reactor for hydrothermal oxidation reaction to prepare oxidized weathered coal;
and step 3: putting the oxidized weathered coal and the second part of water in the step 2 into a reaction kettle, uniformly stirring, adding sodium hydroxide and nano zinc oxide, and performing catalytic hydrolysis and extraction reaction to prepare a sodium humate solution;
and 4, step 4: adding sodium hydroxymethyl sulfonate into the sodium humate solution obtained in the step 3 to perform sulfomethylation reaction;
and 5: and (3) adding dimethyldiallylammonium chloride into the solution subjected to sulfomethylation reaction in the step (4) for crosslinking reaction, pumping the material subjected to crosslinking reaction into a settling tank for settling, concentrating, drying and crushing the settled solution to be less than 0.5 mm.
The weathered coal powder with low humic acid content in the step 2 is crushed to 40-60 meshes, and the mass ratio of the weathered coal with low humic acid content to the first part of water is as follows: 1: 3. the reaction temperature of the hydrothermal oxidizer in the step 2 is 200 ℃, the pressure is 1.8MPa, and the mixed materials are reacted for 30 minutes under the conditions. The mass ratio of the oxidized weathered coal to the second part of water in the step 3 is 1: 6; the mass ratio of the oxidized weathered coal to the sodium hydroxide is 1: 0.15; the mass ratio of the oxidized weathered coal to the nano zinc oxide is 1: 0.002; the temperature of the reaction kettle after the sodium hydroxide and the nano zinc oxide are added is as follows: the reaction was carried out at 130 ℃ for 35 minutes with continuous stirring at 120 rpm. The mass ratio of the addition amount of the sodium hydroxymethyl sulfonate to the oxidized weathered coal in the step 4 is as follows: 0.12: 1; the sulfomethylation reaction is carried out at the temperature of: continuously stirring and reacting for 2 hours at the temperature of 170 ℃; the stirring rate was 120 rpm. The mass ratio of the addition amount of the dimethyl diallyl ammonium chloride to the oxidized weathered coal in the step 5 is as follows: 0.13: 1; before adding dimethyl diallyl ammonium chloride for crosslinking reaction, firstly cooling the solution subjected to sulfomethylation reaction to 70 ℃; the crosslinking reaction was carried out for 25 minutes at a stirring rate of 120 rpm. The concentration in the step 5 is to concentrate the mixture to a solid content of 20% in an environment with a temperature of 75 ℃; the drying is carried out at the temperature of 85-90 ℃ until the water content is 11.5%.
The above examples are merely illustrative for clearly illustrating the present invention and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art upon reference to the above description. It is not necessary or necessary to exhaustively enumerate all embodiments herein, and obvious variations or modifications can be made without departing from the scope of the invention as claimed.
Experimental example:
the high-temperature resistant sodium humate filtrate reducer prepared in example 1 was randomly selected for performance test experiments:
preparing a base slurry solution: 0.79g (weighed to be 0.01g) of anhydrous sodium carbonate and 22.5g (weighed to be 0.01g) of bentonite for a drilling fluid test slurry are added into a beaker containing 350mL of distilled water, stirred at a high speed for 20 minutes, at least two times of the stirring is interrupted during the stirring to scrape off a sample adhered to the cup wall, and the sample is sealed and maintained at 25 +/-1 ℃ for 24 hours to be used as a base slurry.
Test 1: the filtrate loss performance and viscosity of the high-temperature resistant sodium humate filtrate loss reducer prepared in example 1 are measured:
a10.5 g (weighed to 0.01g) sample of the high-temperature fluid loss additive sodium humate is added into 350mL of the base slurry, and the mixture is stirred at a high speed for 20min, wherein the sample adhered to the wall of the cup is scraped off at least twice. The slurry was transferred to a high temperature tank, hot rolled at 180 ℃ for 16 hours, cooled to room temperature, stirred at high speed for 5 minutes, and the apparent viscosity at 24. + -. 3 ℃, API [ (24. + -. 3 ℃)/690kPa ] filtrate loss, and high temperature and high pressure (150 ℃/3450kPa) filtrate loss were measured according to the GB/T16783.1, and the results are shown in Table 1.
TABLE 1 apparent viscosity and fluid loss Performance of fluid loss additives after high temperature aging
From table 1, it can be seen that the apparent viscosity and the filtrate loss reduction of the slurry are within the index requirements, which indicates that the sodium humate has better filtrate loss reduction performance and apparent viscosity at 180 ℃.
And (3) testing 2: evaluation of salt resistance of the high temperature resistant sodium humate fluid loss additive prepared in example 1
Taking 350mL of base slurry, adding 17.5g (weighed to 0.01g) of a sodium humate sample used as a high-temperature-resistant fluid loss additive for drilling fluid and prepared in the test, stirring at a high speed for 20 minutes, at least interrupting twice during the stirring to scrape off the sample adhered to the cup wall, adding 52.5g (weighed to 0.01g) of sodium chloride, stirring at a high speed for 10 minutes, adding 2mL of 20% sodium hydroxide solution and adjusting the pH. The slurry was transferred to a high temperature tank, hot rolled at 180 ℃ for 16 hours, cooled to room temperature, stirred at high speed for 5 minutes, and the apparent viscosity at 24. + -. 3 ℃, API [ (24. + -. 3 ℃)/690kPa ] filtrate loss, and high temperature and high pressure (150 ℃/3450kPa) filtrate loss were measured according to the GB/T16783.1, and the results are shown in Table 2.
TABLE 2 filtrate reducer high temperature aging salt viscosity resistance and filtrate reduction performance
As can be seen from Table 2, the apparent viscosity and the filtrate loss reduction of the 150g/L sodium chloride polluted slurry are within the index requirements, which shows that the sodium humate has better salt resistance at 180 ℃.
Claims (8)
1. A high temperature resistant fluid loss additive sodium humate for well drilling, which is characterized in that: the sodium humate filtrate reducer is prepared from the following raw materials: weathered coal with low humic acid content, sodium hydroxymethyl sulfonate, sodium hydroxide, nano zinc oxide, dimethyl diallyl ammonium chloride and water;
the weathered coal with low humic acid content is weathered coal with humic acid content of 40-50%.
2. The preparation method of the high-temperature-resistant fluid loss additive sodium humate for well drilling according to claim 1, which is characterized by comprising the following steps: the preparation method comprises the following steps:
step 1: dividing water into two parts, namely a first part of water and a second part of water;
step 2: crushing weathered coal with low humic acid content, mixing the crushed weathered coal with first part of water, feeding the mixture into a hydrothermal oxidation reactor, and carrying out hydrothermal oxidation reaction to obtain oxidized weathered coal;
and step 3: putting the oxidized weathered coal and the second part of water in the step 2 into a reaction kettle, uniformly stirring, adding sodium hydroxide and nano zinc oxide, and performing catalytic hydrolysis and extraction reaction to prepare a sodium humate solution;
and 4, step 4: adding sodium hydroxymethyl sulfonate into the sodium humate solution obtained in the step 3 to perform sulfomethylation reaction;
and 5: and (3) adding dimethyldiallylammonium chloride into the solution subjected to sulfomethylation reaction in the step (4) for crosslinking reaction, pumping the material subjected to crosslinking reaction into a settling tank for settling, concentrating, drying and crushing the settled solution to be less than 0.5 mm.
3. The method for preparing the high-temperature-resistant fluid loss additive sodium humate for well drilling according to claim 2, which is characterized in that: the weathered coal powder with low humic acid content in the step 2 is crushed to 40-60 meshes, and the mass ratio of the weathered coal with low humic acid content to the first part of water is as follows: 1: 3.
4. the preparation method of the high-temperature-resistant fluid loss additive sodium humate for drilling according to claim 2, which is characterized in that: the reaction temperature of the hydrothermal oxidizer in the step 2 is 200 ℃, the pressure is 1.8MPa, and the mixed materials are reacted for 30 minutes under the conditions.
5. The preparation method of the high-temperature-resistant fluid loss additive sodium humate for drilling according to claim 2, which is characterized in that: the mass ratio of the oxidized weathered coal to the second part of water in the step 3 is 1: 6; the mass ratio of the oxidized weathered coal to the sodium hydroxide is 1: 0.1-0.2; the mass ratio of the oxidized weathered coal to the nano zinc oxide is 1: 0.001-0.003; the temperature of the reaction kettle after the sodium hydroxide and the nano zinc oxide are added is as follows: and reacting for 30-40 minutes at 130 ℃ under the condition of continuously stirring at 120 revolutions per minute.
6. The preparation method of the high-temperature-resistant fluid loss additive sodium humate for drilling according to claim 2, which is characterized in that: the mass ratio of the addition amount of the sodium hydroxymethyl sulfonate to the oxidized weathered coal in the step 4 is as follows: 0.05-0.2: 1;
the sulfomethylation reaction is carried out at the temperature of: continuously stirring and reacting for 2 hours at the temperature of 160-180 ℃; the stirring rate was 120 rpm.
7. The preparation method of the high-temperature-resistant fluid loss additive sodium humate for drilling according to claim 2, which is characterized in that: the mass ratio of the addition amount of the dimethyl diallyl ammonium chloride to the oxidized weathered coal in the step 5 is as follows: 0.1-0.15: 1;
before adding dimethyl diallyl ammonium chloride for crosslinking reaction, firstly cooling the solution subjected to sulfomethylation reaction to 60-80 ℃; and reacting for 20-30 minutes at a stirring speed of 120 revolutions per minute during the crosslinking reaction.
8. The preparation method of the high-temperature-resistant fluid loss additive sodium humate for drilling according to claim 2, which is characterized in that: the concentration in the step 5 is carried out at the temperature of 70-80 ℃ until the solid content is 18-22%; and the drying is carried out at the temperature of 85-90 ℃ until the water content is lower than 12%.
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| CN101220260A (en) * | 2007-01-08 | 2008-07-16 | 北京化工大学 | Method of producing novel sulfonation humic acid drilling mud modifying agent |
| CN104031273A (en) * | 2013-03-05 | 2014-09-10 | 新疆双龙腐植酸有限公司 | Method for improving yield of humic acid salt prepared from weathered coal |
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