CN115746821A - Fracturing flowback fluid gel breaker and preparation method thereof - Google Patents
Fracturing flowback fluid gel breaker and preparation method thereof Download PDFInfo
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- 239000012530 fluid Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims abstract description 26
- 239000005708 Sodium hypochlorite Substances 0.000 claims abstract description 15
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 15
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims abstract description 15
- CEJLBZWIKQJOAT-UHFFFAOYSA-N dichloroisocyanuric acid Chemical compound ClN1C(=O)NC(=O)N(Cl)C1=O CEJLBZWIKQJOAT-UHFFFAOYSA-N 0.000 claims abstract description 13
- 235000010288 sodium nitrite Nutrition 0.000 claims abstract description 13
- XSXSKSKONCDOMZ-UHFFFAOYSA-N sodium;1,3,5-trichloro-1,3,5-triazinane-2,4,6-trione Chemical compound [Na+].ClN1C(=O)N(Cl)C(=O)N(Cl)C1=O XSXSKSKONCDOMZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 230000015556 catabolic process Effects 0.000 claims abstract description 10
- 238000006731 degradation reaction Methods 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 8
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims description 54
- 238000003756 stirring Methods 0.000 claims description 44
- 238000006243 chemical reaction Methods 0.000 claims description 28
- 229920002907 Guar gum Polymers 0.000 claims description 27
- 239000000665 guar gum Substances 0.000 claims description 27
- 229960002154 guar gum Drugs 0.000 claims description 27
- 235000010417 guar gum Nutrition 0.000 claims description 27
- 239000000243 solution Substances 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 17
- 230000008961 swelling Effects 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 12
- OTPBAANTTKRERC-UHFFFAOYSA-N benzyl(dodecyl)azanium;chloride Chemical group Cl.CCCCCCCCCCCCNCC1=CC=CC=C1 OTPBAANTTKRERC-UHFFFAOYSA-N 0.000 claims description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- 102100032487 Beta-mannosidase Human genes 0.000 claims description 6
- 101710121765 Endo-1,4-beta-xylanase Proteins 0.000 claims description 6
- 108090000790 Enzymes Proteins 0.000 claims description 6
- 102000004190 Enzymes Human genes 0.000 claims description 6
- 102000006995 beta-Glucosidase Human genes 0.000 claims description 6
- 108010047754 beta-Glucosidase Proteins 0.000 claims description 6
- 108010055059 beta-Mannosidase Proteins 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 230000000630 rising effect Effects 0.000 claims description 6
- 101710152845 Arabinogalactan endo-beta-1,4-galactanase Proteins 0.000 claims description 3
- 101710147028 Endo-beta-1,4-galactanase Proteins 0.000 claims description 3
- 239000007853 buffer solution Substances 0.000 claims description 3
- XPFJYKARVSSRHE-UHFFFAOYSA-K trisodium;2-hydroxypropane-1,2,3-tricarboxylate;2-hydroxypropane-1,2,3-tricarboxylic acid Chemical compound [Na+].[Na+].[Na+].OC(=O)CC(O)(C(O)=O)CC(O)=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O XPFJYKARVSSRHE-UHFFFAOYSA-K 0.000 claims description 3
- 108010066429 galactomannanase Proteins 0.000 claims 1
- 239000000654 additive Substances 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 description 4
- 239000007800 oxidant agent Substances 0.000 description 4
- 239000012286 potassium permanganate Substances 0.000 description 4
- 239000002775 capsule Substances 0.000 description 3
- 239000011162 core material Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- OMDQUFIYNPYJFM-XKDAHURESA-N (2r,3r,4s,5r,6s)-2-(hydroxymethyl)-6-[[(2r,3s,4r,5s,6r)-4,5,6-trihydroxy-3-[(2s,3s,4s,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxyoxan-2-yl]methoxy]oxane-3,4,5-triol Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@@H]1OC[C@@H]1[C@@H](O[C@H]2[C@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O)[C@H](O)[C@H](O)[C@H](O)O1 OMDQUFIYNPYJFM-XKDAHURESA-N 0.000 description 2
- 229920000926 Galactomannan Polymers 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- JGJLWPGRMCADHB-UHFFFAOYSA-N hypobromite Chemical compound Br[O-] JGJLWPGRMCADHB-UHFFFAOYSA-N 0.000 description 2
- 239000003094 microcapsule Substances 0.000 description 2
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 239000002562 thickening agent Substances 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000003129 oil well Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 235000000346 sugar Nutrition 0.000 description 1
- 150000008163 sugars Chemical class 0.000 description 1
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Abstract
The invention provides a fracturing flow-back fluid gel breaker and a preparation method thereof, and particularly relates to the technical field of chemical additives, wherein the fracturing flow-back fluid gel breaker is prepared by processing the following raw materials in parts by weight: sodium dichloroisocyanurate: 8 to 15 parts; sodium trichloroisocyanurate: 4 to 10 parts; sodium hypochlorite: 5 to 15 parts; sodium nitrite: 2~6 parts; 5-15 parts of ammonium persulfate; 18-30 parts of a catalyst; auxiliary agent: 3 to 10 parts of the fracturing flowback fluid gel breaker still has high degradation efficiency at normal temperature, and meanwhile, the manufacturing cost is lower.
Description
Technical Field
The invention relates to the technical field of chemical additives, and particularly relates to a fracturing flow-back fluid gel breaker and a preparation method thereof.
Background
In the field of petroleum, fracturing refers to a method for forming cracks on an oil-gas layer by utilizing the hydraulic action in the process of oil extraction or gas production, fracturing is one of main measures for increasing the yield of a gasoline well, the fracturing construction process is that high-viscosity fracturing fluid is pressed into a stratum by utilizing a high-pressure pump set through the principle of liquid pressure transmission, the cracks are formed and a propping agent is carried in, the fracturing fluid injected after the fracturing construction is finished can be largely discharged back to the opposite side, the fracturing fluid is generally called fracturing flowback fluid, the environment can be polluted by returning the flowback fluid to the ground in a large amount, the components of the unconventional fracturing flowback fluid are complex, the types of chemical agents are various, the flowing-back fluid has high COD and high viscosity (the COD can reach 2000-20000mg/L and the viscosity is 8-65 mPa.s), and the characteristic of high stability is realized, so that the gel breaking treatment is usually required before the fracturing flowback fluid is treated, namely, the stability of the flowing-back fluid is required to be destroyed.
The gel breaking principle of the gel breaker is mainly that the molecular chain structure of a thickening agent is broken, so that the viscosity of the thickening agent is reduced and the gel breaker is hydrated, the gel breaker is realized, the common methods for gel breaking comprise a biological method and a chemical method, the biological enzyme gel breaker is green and environment-friendly, but has the problems of slow gel breaking speed and incomplete gel breaking, and can not meet the requirements of gel breaking, the chemical method mainly adopts an oxidation gel breaker method to carry out pretreatment on the gel breaker, and potassium permanganate, sodium hypochlorite, potassium persulfate, ammonium persulfate, hydrogen peroxide and other oxidants are commonly used, for example, the application No. 200410097105.X discloses a microcapsule gel breaker and a preparation method thereof, wherein the microcapsule gel breaker comprises a capsule core material, a coating and an additive, the weight ratio of the capsule core material to the coating to the additive is 85.5-91.2% to 8-13% to 0.8-1.5%, and the capsule core material comprises a single component or a combination of hypochlorite, a hypobromite, a potassium permanganate and potassium dichromate; the preparation method comprises the process steps of adding the raw materials into a side-spraying fluidized bed, adding a binder solution, starting the side-spraying fluidized bed and the like, namely the gel breaking of the return liquid is completed through oxidants such as potassium permanganate, hypochlorite and sulfate, but when the gel breaking is performed through oxidants such as potassium permanganate, sodium hypochlorite, potassium persulfate, ammonium persulfate and hydrogen peroxide, the problem that the gel breaking effect of the oxidants is obviously reduced when the temperature is lower than 50 ℃ easily occurs.
In view of the above, the fracturing flow-back fluid gel breaker and the preparation method thereof provided by the invention still have a remarkable gel breaking effect at a low temperature, can achieve the purpose of rapid gel breaking, are environment-friendly in raw materials and low in cost, and can realize industrial application.
Disclosure of Invention
The invention provides a fracturing flow-back fluid gel breaker and a preparation method thereof, aiming at solving the problems of slow gel breaking speed and incomplete gel breaking of flow-back fluid at low temperature.
The invention is realized by the following technical scheme:
the invention provides a fracturing flow-back fluid gel breaker and a preparation method thereof, wherein the fracturing flow-back fluid gel breaker is prepared by processing the following raw materials in parts by weight:
sodium dichloroisocyanurate: 8 to 15 parts;
sodium trichloroisocyanurate: 4 to 10 parts;
sodium hypochlorite: 5 to 15 parts;
sodium nitrite: 2~6 parts;
5-15 parts of ammonium persulfate;
18-30 parts of a catalyst;
auxiliary agent: 3 to 10 portions.
Further, the preparation method of the fracturing flow-back fluid gel breaker comprises the following steps:
s1, adding sodium dichloroisocyanurate, sodium trichloroisocyanurate and sodium hypochlorite into a reaction kettle according to a certain weight part, stirring for 10min under normal pressure, and introducing ammonia gas for 5min to obtain a mixture A;
s2, continuously stirring the mixture A, adding a certain weight part of sodium nitrite and ammonium persulfate, continuously stirring, heating the reaction kettle to a first preset temperature, and reacting the mixture A for 1 to 2h to obtain a mixture B;
s3, continuously stirring the mixture B, adding a catalyst, continuously stirring, heating the reaction kettle to a second preset temperature, and reacting the mixture B for 3-4 h to obtain a mixture c;
and S4, continuously stirring the mixture C, cooling the mixture C in the reaction kettle to room temperature, and then adding an auxiliary agent to continuously stir for 40min to obtain the fracturing flow-back fluid gel breaker.
Further, the catalyst is a galactomannase solution.
Furthermore, the auxiliary agent is dodecyl benzyl ammonium chloride.
Further, the stirring speed of the reaction kettle is 120r/min.
Further, the preparation method of the galactomannase solution comprises the following steps:
fully mixing guar gum powder with mannase, xylanase and cellobiase to obtain a mixed solution; adding citric acid-sodium citrate buffer solution to prepare guar gum and mixing the guar gum with the mixed solution;
after swelling guar gum, controlling enzymolysis temperature and time to degrade to obtain galactanase solution.
Further, the guar gum powder, the mannase, the xylanase and the cellobiase respectively comprise the following components in parts by weight: 1 part, 50 to 70 parts, 1000 to 3000 parts and 1000 to 2000 parts.
Further, the guar gum is swollen and then is subjected to enzymolysis at a single temperature: the enzymolysis temperature is 50 to 55 ℃, and the time is 6 to 10 hours.
Further, a temperature gradient enzyme degradation mode is adopted after swelling, and the degradation steps are as follows:
raising the temperature from the swelling temperature to 35 to 40 ℃, and carrying out enzymolysis for 1.5 to 2.5 hours;
raising the temperature to 48-53 ℃, and carrying out enzymolysis for 3-4h; increasing 1~2 ℃ every 3~5 minutes in the temperature rising process, and keeping for 10 minutes every 1~2 ℃ in the temperature rising process;
the temperature is raised to 55 ℃, and enzymolysis is carried out for 2 to 3 hours.
Further, the concentration of the guar gum solution is 8-12%, the swelling time is 30-90min, and the swelling temperature is 26-38 ℃.
The invention has the beneficial effects that:
the fracturing flowback fluid gel breaker provided by the invention still has a high gel breaking speed at normal temperature, the used raw materials are environment-friendly and low in cost, the industrial application can be realized, meanwhile, the gel breaker can rapidly break the bottom of the guar gum in the flowback fluid in a short time through the galactomannan enzyme, and the degradation rate is high.
Drawings
FIG. 1 is a graph comparing the fracture rate of the fracturing flow-back fluid gel breaker of the invention with that of a market product at 20 ℃;
FIG. 2 is a graph comparing the fracture flowback fluid breaker of the invention with the fracture flowback fluid breaker of the market products at 30 ℃;
FIG. 3 is a graph comparing the fracture flow-back fluid breaker of the present invention with the fracture flow-back fluid breaker of the market products at 40 ℃;
fig. 4 is a flow chart of the preparation of the fracturing flowback fluid gel breaker of the invention.
The implementation, functional features and advantages of the present invention will be further described with reference to the accompanying drawings.
Detailed Description
In order to more clearly and completely describe the technical scheme of the invention, the invention is further described with reference to the accompanying drawings.
Referring to fig. 1 to fig. 3, the invention provides a fracturing flow-back fluid gel breaker prepared from the following raw materials in parts by weight:
sodium dichloroisocyanurate: 8 to 15 parts;
sodium trichloroisocyanurate: 4 to 10 parts;
sodium hypochlorite: 5 to 15 parts;
sodium nitrite: 2~6 parts;
5-15 parts of ammonium persulfate;
18-30 parts of a catalyst;
auxiliary agent: 3 to 10 portions.
The preparation method of the fracturing flow-back fluid gel breaker comprises the following steps:
s1, adding sodium dichloroisocyanurate, sodium trichloroisocyanurate and sodium hypochlorite into a reaction kettle according to a certain weight part, stirring for 10min under normal pressure, and introducing ammonia gas for 5min to obtain a mixture A;
s2, continuously stirring the mixture A, adding a certain weight part of sodium nitrite and ammonium persulfate, continuously stirring, heating the reaction kettle to a first preset temperature, and reacting the mixture A for 1 to 2h to obtain a mixture B;
s3, continuously stirring the mixture B, adding the galactomannan enzyme solution, continuously stirring, heating the reaction kettle to a second preset temperature, and reacting the mixture B for 3-4 h to obtain a mixture c;
and S4, continuously stirring the mixture C, cooling the mixture C in the reaction kettle to room temperature, and then adding dodecyl benzyl ammonium chloride to continuously stir for 40min to obtain the fracturing flow-back fluid gel breaker.
In one embodiment, the first preset temperature is 55-65 ℃, the second preset temperature is 70-80 ℃, the reaction temperature can be controlled according to the actual situation in the specific implementation, and can be 56 ℃ or 60 ℃, wherein the galactomannase has the capability of catalyzing the breakage of glycosidic bonds in the flowback liquid to form small molecular sugars, so that the purpose of breaking the gum is achieved, meanwhile, a large amount of substrates such as guar gum and the like exist in the flowback liquid, and the galactomannase only participates in the reaction process because the galactomannase is unchanged before and after the degradation of the guar gum, so that the galactomannase can thoroughly degrade a large amount of substrates such as guar gum and the like in the flowback liquid at a low concentration in a short time.
In one embodiment, the process for preparing the galactomannase solution comprises the steps of:
fully mixing guar gum powder with mannase, xylanase and cellobiase to obtain a mixed solution;
wherein the guar gum powder, the mannase, the xylanase and the cellobiase are respectively prepared from the following components in parts by weight: 1 part of: 50 to 70 parts: 1000 to 3000 parts: 1000 to 2000 parts; adding citric acid-sodium citrate buffer solution to prepare guar gum and mixing the guar gum with the mixed solution; after swelling guar gum, controlling enzymolysis temperature and time to degrade to obtain galactanase solution.
Wherein the concentration of the guar gum solution is 8 to 12 percent, the swelling time is 30 to 90min, and the swelling temperature is 26 to 38 ℃.
After swelling, guar gum can be degraded by one of the following two degradation modes:
the first method comprises the following steps: and (3) swelling guar gum, and then performing enzymolysis at a single temperature: the enzymolysis temperature is 50 to 55 ℃, and the time is 6 to 10 hours;
and the second method comprises the following steps: after swelling guar gum, degrading by adopting a temperature gradient enzyme degradation mode, wherein the degradation step is as follows:
raising the temperature from the swelling temperature to 35 to 40 ℃, and carrying out enzymolysis for 1.5 to 2.5 hours;
raising the temperature to 48-53 ℃, and carrying out enzymolysis for 3-4h; increasing 1~2 ℃ every 3~5 minutes in the temperature rising process, and keeping for 10 minutes every 1~2 ℃ in the temperature rising process;
the temperature is raised to 55 ℃, and enzymolysis is carried out for 2 to 3 hours.
Referring to the attached figures 1-3, examples 1-3 of the fracturing fluid-repellent breaker of the invention are shown in comparison with a commercial product.
Example 1:
the fracturing flow-back fluid gel breaker is prepared by processing the following raw materials in parts by weight: 8 parts of sodium dichloroisocyanurate, 4 parts of sodium trichloroisocyanurate, 5 parts of sodium hypochlorite, 2 parts of sodium nitrite, 5 parts of ammonium persulfate, 18 parts of galactomannase solution and 3 parts of dodecyl benzyl ammonium chloride.
The specific preparation process comprises the following steps:
s1, adding sodium dichloroisocyanurate, sodium trichloroisocyanurate and sodium hypochlorite into a reaction kettle according to a certain weight part, stirring for 10min under normal pressure, and introducing ammonia gas for 5min to obtain a mixture A;
s2, continuously stirring the mixture A, adding a certain weight part of sodium nitrite and ammonium persulfate, continuously stirring, heating the reaction kettle to 55-65 ℃, and reacting the mixture A for 1h to obtain a mixture B;
s3, continuously stirring the mixture B, adding a prepared galactomannase solution, continuously stirring, heating the reaction kettle to 70-80 ℃, and reacting the mixture B for 3 hours to obtain a mixture c;
and S4, continuously stirring the mixture C, cooling the mixture C in the reaction kettle to room temperature, and then adding dodecyl benzyl ammonium chloride to continuously stir for 40min to obtain the fracturing flow-back fluid gel breaker.
Example 2:
the fracturing flow-back fluid gel breaker is prepared by processing the following raw materials in parts by weight: 12 parts of sodium dichloroisocyanurate, 6 parts of sodium trichloroisocyanurate, 10 parts of sodium hypochlorite, 4 parts of sodium nitrite, 10 parts of ammonium persulfate, 22 parts of galactomannase solution and 7 parts of dodecyl benzyl ammonium chloride.
The specific preparation process comprises the following steps:
s1, adding sodium dichloroisocyanurate, sodium trichloroisocyanurate and sodium hypochlorite into a reaction kettle according to a certain weight part, stirring for 10min under normal pressure, and introducing ammonia gas for 5min to obtain a mixture A;
s2, continuously stirring the mixture A, adding a certain weight part of sodium nitrite and ammonium persulfate, continuously stirring, heating the reaction kettle to 55-65 ℃, and reacting the mixture A for 1.5h to obtain a mixture B;
s3, continuously stirring the mixture B, adding a prepared galactomannase solution, continuously stirring, heating the reaction kettle to 70-80 ℃, and reacting the mixture B for 3.5 hours to obtain a mixture c;
and S4, continuously stirring the mixture C, cooling the mixture C in the reaction kettle to room temperature, and then adding dodecyl benzyl ammonium chloride to continuously stir for 40min to obtain the fracturing flow-back fluid gel breaker.
Example 3:
the fracturing flow-back fluid gel breaker is prepared by processing the following raw materials in parts by weight: 15 parts of sodium dichloroisocyanurate, 10 parts of sodium trichloroisocyanurate, 15 parts of sodium hypochlorite, 6 parts of sodium nitrite, 15 parts of ammonium persulfate, 30 parts of galactomannase solution and 10 parts of dodecyl benzyl ammonium chloride.
S1, adding sodium dichloroisocyanurate, sodium trichloroisocyanurate and sodium hypochlorite into a reaction kettle according to a certain weight part, stirring for 10min under normal pressure, and introducing ammonia gas for 5min to obtain a mixture A;
s2, continuously stirring the mixture A, adding a certain weight part of sodium nitrite and ammonium persulfate, continuously stirring, heating the reaction kettle to 55-65 ℃, and reacting the mixture A for 2 hours to obtain a mixture B;
s3, continuously stirring the mixture B, adding a prepared galactomannase solution, continuously stirring, heating the reaction kettle to 70-80 ℃, and reacting the mixture B for 4 hours to obtain a mixture c;
and S4, continuously stirring the mixture C, cooling the mixture C in the reaction kettle to room temperature, and then adding dodecyl benzyl ammonium chloride to continuously stir for 40min to obtain the fracturing flow-back fluid gel breaker.
The performance of the fracturing flow-back fluid gel breaker obtained in the embodiment 1-3 and the commercially available product 1-2 is detected, and the detection method is as follows:
the initial viscosity of the flowback fluid of the fracturing flow-back fluid of a certain oil field oil well is 45.2 mPa.s. The fracturing flow-back fluid is taken and added with the gel breaker and the products sold in the market 1-2 respectively, the weight proportion of the gel breaker in the fracturing flow-back fluid is 5.0%, and the gel breaking performance of the gel breaker under the conditions of 20 ℃, 30 ℃ and 40 ℃ is tested, so that the test results shown in the figures 1-3 are obtained.
As can be seen from the experimental result tables in fig. 1 to 3, as the temperature rises and the gel breaking time is prolonged, the fracturing flow-back fluid is reduced in years, the gel breaking effect is better, and under the condition of 40 ℃, the viscosity of the fracturing flow-back fluid of examples 1 to 3 is reduced to be less than 3.2mpa.s, and the viscosity is reduced by more than 92.52% when the gel breaking time reaches 30 min.
Of course, the present invention may have other embodiments, and based on the embodiments, those skilled in the art can obtain other embodiments without any creative effort, and all of them are within the protection scope of the present invention.
Claims (10)
1. The fracturing flow-back fluid gel breaker is characterized by being prepared from the following raw materials in parts by weight:
sodium dichloroisocyanurate: 8 to 15 parts;
sodium trichloroisocyanurate: 4 to 10 parts;
sodium hypochlorite: 5 to 15 parts;
sodium nitrite: 2~6 parts;
5-15 parts of ammonium persulfate;
18-30 parts of a catalyst;
auxiliary agent: 3 to 10 portions.
2. The preparation method of the fracturing flow-back fluid gel breaker is characterized by comprising the following steps of:
s1, adding sodium dichloroisocyanurate, sodium trichloroisocyanurate and sodium hypochlorite into a reaction kettle according to a certain weight part, stirring for 10min under normal pressure, and introducing ammonia gas for 5min to obtain a mixture A;
s2, continuously stirring the mixture A, adding a certain weight part of sodium nitrite and ammonium persulfate, continuously stirring, heating the reaction kettle to a first preset temperature, and reacting the mixture A for 1 to 2h to obtain a mixture B;
s3, continuously stirring the mixture B, adding a catalyst, continuously stirring, heating the reaction kettle to a second preset temperature, and reacting the mixture B for 3-4 h to obtain a mixture c;
and S4, continuously stirring the mixture C, cooling the mixture C in the reaction kettle to room temperature, and then adding an auxiliary agent to continuously stir for 40min to obtain the fracturing flow-back fluid gel breaker.
3. The frac flowback fluid breaker of claim 1, wherein the catalyst is a galactomannanase solution.
4. The fracturing flow-back fluid breaker of claim 1, wherein the auxiliary agent is dodecyl benzyl ammonium chloride.
5. The preparation method of the fracturing flow-back fluid breaker as claimed in claim 2, wherein the stirring speed of the reaction kettle is 120r/min.
6. The fracturing flow-back fluid breaker of claim 3, wherein the preparation method of the galactomannase solution comprises the following steps:
fully mixing guar gum powder with mannase, xylanase and cellobiase to obtain a mixed solution; adding citric acid-sodium citrate buffer solution to prepare guar gum and mixing the guar gum with the mixed solution;
after swelling guar gum, controlling enzymolysis temperature and time to degrade to obtain galactanase solution.
7. The fracturing flow-back fluid gel breaker and the preparation method thereof according to claim 6, wherein the guar gum powder, the mannase, the xylanase and the cellobiase are respectively prepared from the following components in parts by weight: 1 part, 50 to 70 parts, 1000 to 3000 parts and 1000 to 2000 parts.
8. The fracturing flow-back fluid gel breaker and the preparation method thereof according to claim 6, wherein the guar gum is swelled and then subjected to enzymolysis at a single temperature: the enzymolysis temperature is 50 to 55 ℃, and the time is 6 to 10 hours.
9. The fracturing flow-back fluid gel breaker and the preparation method thereof as claimed in claim 6, wherein a temperature gradient enzyme degradation mode is adopted after swelling, and the degradation steps are as follows:
increasing the temperature from the swelling temperature to 35 to 40 ℃, and carrying out enzymolysis for 1.5 to 2.5 hours;
raising the temperature to 48-53 ℃, and carrying out enzymolysis for 3-4h; increasing 1~2 ℃ every 3~5 minutes in the temperature rising process, and keeping for 10 minutes every 1~2 ℃ in the temperature rising process;
the temperature is raised to 55 ℃, and enzymolysis is carried out for 2 to 3 hours.
10. The method for preparing the fracturing flowback fluid gel breaker machine according to claim 6, wherein the concentration of the guar gum solution is 8-12%, the swelling time is 30-90min, and the swelling temperature is 26-38 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211518380.9A CN115746821A (en) | 2022-11-30 | 2022-11-30 | Fracturing flowback fluid gel breaker and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101781552A (en) * | 2009-12-21 | 2010-07-21 | 陕西延长石油(集团)有限责任公司研究院 | Bio-enzyme gel breaker and technique for water-based guargum fracturing gel breaking with the same |
| CN104745659A (en) * | 2015-04-14 | 2015-07-01 | 刘云国 | Method for rapidly preparing galactomannan oligosaccharide enzymatic hydrolysate by utilizing guar gum |
| CN106318364A (en) * | 2016-08-23 | 2017-01-11 | 烟台智本知识产权运营管理有限公司 | Compound gel breaker and preparing method thereof |
| CN106318363A (en) * | 2016-08-23 | 2017-01-11 | 烟台智本知识产权运营管理有限公司 | Fracturing recovery fluid gel breaker and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101781552A (en) * | 2009-12-21 | 2010-07-21 | 陕西延长石油(集团)有限责任公司研究院 | Bio-enzyme gel breaker and technique for water-based guargum fracturing gel breaking with the same |
| CN104745659A (en) * | 2015-04-14 | 2015-07-01 | 刘云国 | Method for rapidly preparing galactomannan oligosaccharide enzymatic hydrolysate by utilizing guar gum |
| CN106318364A (en) * | 2016-08-23 | 2017-01-11 | 烟台智本知识产权运营管理有限公司 | Compound gel breaker and preparing method thereof |
| CN106318363A (en) * | 2016-08-23 | 2017-01-11 | 烟台智本知识产权运营管理有限公司 | Fracturing recovery fluid gel breaker and preparation method thereof |
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| 王满学;何静;杨志刚;尚文静;王建民;: "生物酶SUN-1/过硫酸铵对羟丙基瓜胶压裂液破胶和降解作用", 西安石油大学学报(自然科学版), no. 01, pages 74 - 75 * |
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