CN113356790B - Low-temperature shallow well cementing method - Google Patents
Low-temperature shallow well cementing method Download PDFInfo
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- CN113356790B CN113356790B CN202110771806.0A CN202110771806A CN113356790B CN 113356790 B CN113356790 B CN 113356790B CN 202110771806 A CN202110771806 A CN 202110771806A CN 113356790 B CN113356790 B CN 113356790B
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- E—FIXED CONSTRUCTIONS
- E21—EARTH DRILLING; MINING
- E21B—EARTH DRILLING, e.g. DEEP DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B33/00—Sealing or packing boreholes or wells
- E21B33/10—Sealing or packing boreholes or wells in the borehole
- E21B33/13—Methods or devices for cementing, for plugging holes, crevices, or the like
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- 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
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/504—Compositions based on water or polar solvents
- C09K8/506—Compositions based on water or polar solvents containing organic compounds
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- 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
- C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
- C09K8/504—Compositions based on water or polar solvents
- C09K8/506—Compositions based on water or polar solvents containing organic compounds
- C09K8/508—Compositions based on water or polar solvents containing organic compounds macromolecular compounds
- C09K8/512—Compositions based on water or polar solvents containing organic compounds macromolecular compounds containing cross-linking agents
Abstract
The invention relates to a well cementation method of a low-temperature shallow well, which sequentially comprises the following steps: lowering a casing string in a borehole; mounting a cement head on the joint, wherein a rubber plug is arranged in the upper part of the cement head; thirdly, the drilling fluid is conveyed into the inner cavity of the sleeve and flows back to the ground along the annular space of the borehole, and rock debris is cleaned; fourthly, injecting isolation liquid into the sleeve string; fifthly, injecting the well cementation cement slurry into the casing string until the well cementation cement slurry reaches the designed well cementation amount; sixthly, releasing the rubber plug, injecting plugging liquid into the cement vehicle through a plugging liquid inlet, and pushing the plugging liquid to move downwards along with the rubber plug; injecting drilling fluid for replacing slurry, pushing the plug pressing fluid to move downwards by the drilling fluid, pushing the cementing cement slurry to move downwards by the rubber plug, pushing the spacer fluid to move upwards after the cementing cement slurry enters the well hole annulus from the floating shoe, and pushing the drilling fluid to move upwards by the spacer fluid; and when the rubber plug is moved downwards to the flow blocking plate of the float collar, collision pressure is generated, the slurry pump is immediately turned off, and the cement slurry is raised to a preset well section to enter a coagulation waiting state. The invention has good safety, high construction success rate and good well cementation quality.
Description
Technical Field
The invention relates to oil and gas well cementation, in particular to a well cementation method of a low-temperature shallow well, and belongs to the technical field of oil and gas well cementation.
Background
The oil well cement used in the existing well cementation is silicate oil well cement, and has the outstanding problems that the cement paste has long setting time and slow strength development, and particularly under the condition of a low-temperature shallow layer well below 60 ℃, the well is shallow and has low ground temperature, the oil well cement has slow strength development and long setting time, increases the drilling cost, easily causes annular channeling, and influences the well cementation quality and the operation safety. The cement paste is difficult to form high enough strength in the normal waiting time, and cannot meet the production and exploitation requirements. Calcium chloride is usually added as an early strength agent, but the early strength agent has large influence on the rheological property of cement paste, is difficult to mix the cement paste and is not beneficial to pumping.
When cementing, after a well hole and an annulus are cleaned through circulation of drilling fluid, firstly, the pilot spacer fluid is injected into a casing string, then, low-temperature cementing cement slurry is injected to reach the designed cementing amount, and the drilling fluid is separated from the low-temperature cementing cement slurry by the pilot spacer fluid. The fluid loss agent is an important component in low-temperature well cementation cement slurry, and researchers in various countries carry out deep research on additives such as the fluid loss agent and a pilot spacer fluid aiming at the well cementation problem under the low-temperature condition for many years, so that a plurality of novel spacer fluids and additives are developed, abundant research results are obtained, and the low-temperature well cementation technology is greatly developed.
The low-temperature isolating liquid system commonly used at present is mainly a flushing type isolating liquid, the main component is water, and a high-efficiency flushing agent and a tackifier are added into the water, so that the isolating liquid has poor isolating effect, large water loss, low rock debris carrying efficiency and low suspension capacity, and is easy to cause formation damage or failure of well cementation operation.
The common defects of the current common dehydration agent in cement slurry for well cementation are as follows: 1. commonly used in oil well cement fluid loss additives are various cellulose ethers including carboxymethyl cellulose (CMC), hydroxyethyl cellulose (HEC), carboxymethyl hydroxyethyl cellulose (CMHEC), and the like. Cellulose ether polymers have good water loss reducing performance, but the addition of the cellulose materials thickens cement paste, the cement paste is difficult to mix and even pump when the addition amount is high, and the materials have strong retarding effect and delay the strength development of cement stones.
2. At present, the fluid loss additive on the market is used for solving the problem of the performance of the cement paste under the high-temperature condition and lacking in the evaluation of the performance of the cement paste under the low-temperature condition.
3. After the fluid loss agent is transported to a construction site, water distribution is generally carried out first, then an experiment is carried out, and slurry distribution and well cementation are carried out when the experiment indexes are met. However, in the field, due to other factors, the slurry preparation and well cementation are delayed, the waiting time in the field is long, the performance of the fluid loss agent is changed, and the failure of the well cementation is easily caused in serious cases. Therefore, when slurry is actually prepared, the performance of the fluid loss agent needs to be rechecked, and if the rechecking index does not meet the requirement, the fluid loss agent is discarded. In most cases, the delay exceeds one week and is discarded, resulting in waste and increased production cost.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the low-temperature shallow well cementing method which has the advantages of good construction safety, high success rate, fast strength increase and good well cementing quality.
In order to solve the technical problems, the well cementation method of the low-temperature shallow well sequentially comprises the following steps of: the method comprises the steps of running a casing string in a well after the well is communicated, wherein floating shoes are arranged at the bottoms of the casing string, floating hoops are arranged above the floating shoes at intervals of one casing, a joint top section is arranged at the top of the casing string, and drilling fluid is filled in each casing after each casing is run into the well; secondly, a cementing head is installed on the jacking section, a rubber plug is arranged in the upper part of the cementing head, and the bottom of the rubber plug abuts against a rubber plug stop pin; the top of the cement head is provided with a plug pressing liquid inlet, and the side wall of the middle part of the cement head is symmetrically provided with a low-temperature well cementation cement slurry inlet and a drilling liquid inlet; thirdly, the mud pump is started to send the drilling fluid into the inner cavity of the casing, the drilling fluid enters the borehole annulus from the floating shoe at the bottom of the casing, flows back to the ground along the borehole annulus upwards, and the rock debris in the borehole is cleaned to the ground; fourthly, injecting the prepared isolation liquid into the sleeve string by using a cement truck; fifthly, injecting the prepared low-temperature well cementation cement slurry into the casing string by using a cement truck until the low-temperature well cementation cement slurry reaches the designed well cementation amount; sixthly, removing a rubber plug stop pin on the cement head, releasing the rubber plug, injecting plugging liquid into the cement vehicle through a plugging liquid inlet, and pushing the rubber plug to move downwards by the plugging liquid; starting a mud pump, injecting drilling fluid to replace slurry, pushing the plugging fluid to move downwards, pushing the low-temperature well cementation cement slurry to move downwards through a rubber plug, pushing the spacer fluid to move upwards after the low-temperature well cementation cement slurry enters a borehole annulus from a floating shoe, and pushing the drilling fluid to move upwards through the spacer fluid; and when the rubber plug moves downwards to the flow blocking plate of the float collar, collision pressure is generated, the slurry pump is immediately turned off, and at the moment, the low-temperature well cementation cement slurry returns to the preset well section and enters the waiting setting.
Compared with the prior art, the invention has the following beneficial effects: 1. the buoyancy effect of the drilling fluid in the borehole on the casing string in the casing running process can be reduced when every next casing is filled with the drilling fluid, and the casing running can be smoothly carried out; secondly, the whole pipe string is filled with a large amount of air after the slurry is not poured for a long time, and when the circulation of the casing is finished, the air can be pushed into the annular space between the casing and the borehole, so that the pressure of the annular liquid column outside the casing is reduced, and the borehole is easy to collapse. 2. The low-temperature well cementing cement slurry inlet and the drilling fluid inlet of the cementing head are positioned below the rubber plug, and the drilling fluid is circulated to clean the well wall and carry rock debris at the bottom of the well to the ground, so that the annular cleanliness of the well is improved, and the well cementing quality is improved. 3. The spacer fluid is injected before the low-temperature well cementation cement slurry, and the spacer fluid contains a weighting spacer agent and a surfactant, so that on one hand, the effect of isolating the drilling fluid is achieved, and the formation of mixed slurry which influences the well cementation quality of the upper well section due to the direct contact of the low-temperature well cementation cement slurry and the drilling fluid is effectively avoided; on the other hand, the well wall and the outer wall of the casing are cleaned again to ensure that the well is in a cleaner state before the cement is contacted with the well wall, so that the cement is better combined with the well wall and the outer wall of the casing, and the well cementation quality is further improved. 4. The drilling fluid is injected for replacing the slurry, so that the residual low Wen Gujing cement slurry in the casing can be replaced to the outer annular space of the casing, and the low-temperature well cementation cement slurry can reach a preset height return position according to design requirements; in the slurry replacing process, the low-temperature well cementation cement slurry entering the annulus initially can carry out secondary flushing on the well wall so as to ensure that the annulus of the lower well section can be completely filled with the low-temperature well cementation cement slurry, and the purpose of improving the well cementation quality is achieved.
As a preferred embodiment of the present invention, the release liquid of step four has the following raw material components and weight contents, water: 400 parts of suspending agent TAS155:2 parts of surfactant XP-1:4 parts of an anti-collapse release agent JS-1:12-20 parts of barite powder: 180-490 parts.
As a preferred scheme of the invention, the preparation method of the anti-collapse separant JS-1 sequentially comprises the following steps: the preparation method comprises the steps of heating 100 parts of deionized water to 70 ℃, adding 4 parts of octylphenol polyoxyethylene ether, cooling to 60 ℃, adding 18-22 parts of vinyltriethoxysilane, keeping the temperature, stirring for 2 hours, stirring for 20 minutes at a rotating speed of 300-500rpm, stirring for 30 minutes at a rotating speed of 300rpm, and stirring for 150-200rpm at the other time to obtain an organic silicon prepolymerization emulsion; dissolving 2 parts of sodium dodecyl benzene sulfonate in 100 parts of deionized water, then dropwise adding an acrylic acid-acetic monomer, wherein the acrylic acid-acetic monomer is premixed with 9-11 parts of methyl methacrylate, 18-22 parts of butyl acrylate and 4 parts of hydroxyethyl methacrylate, and stirring for 0.5 hour at a rotating speed of more than 300rpm to obtain a pre-emulsion A; thirdly, adding 0.3-0.5 part of potassium persulfate into 100 parts of deionized water to prepare a solution B; stirring the organic silicon pre-polymerization emulsion at the rotating speed of 300rpm, heating to 70 ℃, slowly dropwise adding the pre-emulsion A and the solution B, finishing dropwise adding within 1 hour, heating to 80 ℃, stirring at the rotating speed of 150-200rpm, keeping the temperature for 2 hours, and cooling to below 40 ℃; and fifthly, regulating the pH value to 7-8 by using triethanolamine to obtain the collapse preventing separant JS-1.
As a preferable scheme of the invention, the isolation liquid comprises the following raw material components in percentage by weight: 400 parts of suspending agent TAS155:2 parts of surfactant XP-1:4 parts of an anti-collapse release agent JS-1:12 parts of barite powder: 180 parts of (A); the anti-collapse release agent JS-1 comprises the following raw material components in percentage by weight, and deionized water: 300 parts of octyl phenol polyoxyethylene ether: 4 parts of vinyltriethoxysilane: 18 parts of sodium dodecyl benzene sulfonate: 2 parts of methyl methacrylate: 9 parts of butyl acrylate: 18 parts of hydroxyethyl methacrylate: 4 parts and potassium persulfate: 0.3 part.
As a preferable scheme of the invention, the isolation liquid comprises the following raw material components in percentage by weight: 400 parts of suspending agent TAS155:2 parts of surfactant XP-1:4 parts of an anti-collapse release agent JS-1:16 parts of barite powder: 300 parts of (A); the anti-collapse release agent JS-1 comprises the following raw material components and weight content, deionized water: 300 parts of octyl phenol polyoxyethylene ether: 4 parts of vinyltriethoxysilane: 20 parts of sodium dodecyl benzene sulfonate: 2 parts of methyl methacrylate: 10 parts of butyl acrylate: 20 parts of hydroxyethyl methacrylate: 4 parts and potassium persulfate: 0.4 part.
As a preferable scheme of the invention, the isolation liquid comprises the following raw material components in percentage by weight: 400 parts of suspending agent TAS155:2 parts of surfactant XP-1:4 parts of an anti-collapse release agent JS-1:20 parts of barite powder: 490 parts; the anti-collapse release agent JS-1 comprises the following raw material components and weight content, deionized water: 300 parts of octyl phenol polyoxyethylene ether: 4 parts of vinyltriethoxysilane: 22 parts of sodium dodecyl benzene sulfonate: 2 parts of methyl methacrylate: 11 parts and butyl acrylate: 22 parts of hydroxyethyl methacrylate: 4 parts and potassium persulfate: 0.5 part.
The spacer fluid of the invention has the following beneficial effects: 1. the suspending agent TAS155 can increase the viscosity and the suspension performance of the spacer fluid, form a certain viscosity difference with the drilling fluid, and is beneficial to the later-stage displacement efficiency; the surfactant XP-1 can eliminate bubbles generated in the preparation process of the spacer fluid; the anti-collapse release agent JS-1 can increase the compatibility among the drilling fluid, the release fluid and the cement paste, and avoid the occurrence of accelerated setting after the mixing of the drilling fluid, the release fluid and the cement paste, which leads to the construction failure; the barite powder is used to pre-adjust the density of the spacer fluid. 2. The prevalence index of the spacer fluid is less than 0.7, the spacer fluid has good advantages in rheology and mud cake carrying, has good collapse resistance, and can protect the safety of well construction; 3. the flushing efficiency of the oil-based drilling fluid is up to more than 97%, loose mud cakes on a well wall and a casing can be more effectively flushed, the well can be further cleaned, and the cementing strength of a cement sheath and a first cementing surface of the casing and a second cementing surface of the well can be improved; 4. the drilling fluid has good rheological property under the condition of low temperature and good rheological property, and is beneficial to displacing the drilling fluid.
As a preferred scheme of the invention, the preparation of the low-temperature well cementation cement slurry prepared in the step fifthly sequentially comprises the following steps: pouring 4.8-12 parts of fluid loss additive and 2.4 parts of dispersant USZ into 352 parts of deionized water and stirring uniformly; step b: mixing 800 parts of G-grade oil well cement, 16-24 parts of calcium chloride and 32-40 parts of silica fume in a dry powder manner; step c: b, putting the mixed dry powder in the step b into the solution in the step a, and uniformly stirring to obtain low-temperature well cementing cement slurry; the preparation method of the fluid loss agent sequentially comprises the following steps: (1) 6-8 parts of polyvinyl alcohol PVA1788 is dissolved in 100 parts of deionized water to prepare a polyvinyl alcohol aqueous solution; (2) adding 10-13 parts of cross-linking agent glutaraldehyde into polyvinyl alcohol aqueous solution, stirring for 20-30 minutes, and heating to 50-60 ℃ while stirring; (3) adjusting the pH value to 4-5 with concentrated hydrochloric acid, continuously stirring for reaction for 1 hour, and carrying out chemical reaction under an acidic condition; (4) and adjusting the pH value to 7-8 by using NaOH solution, cooling to room temperature, adding 1-1.5 parts of formaldehyde solution, and uniformly mixing to obtain the fluid loss agent.
As a preferred scheme of the invention, the weight content of part of raw materials is as follows: 4.8 parts of calcium chloride: 16 parts of silica fume: 32 parts of polyvinyl alcohol PVA1788:6 parts of cross-linking agent glutaraldehyde: 10 parts of formaldehyde: 1 part.
As a preferred scheme of the invention, the weight content of part of raw materials is as follows: 8 parts of calcium chloride: 20 parts of micro silicon powder: 36 parts of polyvinyl alcohol PVA1788:7 parts of cross-linking agent glutaraldehyde: 11 parts and formaldehyde: 1.2 parts.
As a preferable scheme of the invention, the weight contents of partial raw materials are as follows: 12 parts of calcium chloride: 24 parts of micro silicon powder: 40 parts of polyvinyl alcohol PVA1788:8 parts of cross-linking agent glutaraldehyde: 13 parts and formaldehyde: 1.5 parts.
The low-temperature well cementation cement slurry has the following beneficial effects: 1. the silica fume is used for ensuring the cement paste to have better rheological property and is convenient for pumping; the calcium chloride has the function of improving the early strength of the cement stone under the low-temperature condition, the polyvinyl alcohol PVA1788 can thicken the cement paste, and the dispersant USZ is used for solving the phenomenon of thickening of the cement paste. 2. Glutaraldehyde and formaldehyde are used as cross-linking agents, and cross-linking reaction is carried out on the glutaraldehyde and the formaldehyde with polyvinyl alcohol PVA1788 to form the fluid loss agent. 3. Aldehyde functional groups are arranged at two ends of glutaraldehyde and can be used as a cross-linking agent, intermolecular and intramolecular cross-linking reactions can be carried out between the glutaraldehyde and the polyvinyl alcohol in the cross-linking process, under the catalytic action of acid, the hydroxyl of the polyvinyl alcohol is connected with the carbonyl of the glutaraldehyde to generate an acetal reaction, and water and polyvinyl acetal are generated; the degree of crosslinking is best at a temperature of 55 ℃.4. Glutaraldehyde provides crosslinking points for polyvinyl alcohol molecules, and polyvinyl alcohol is crosslinked on carbonyl carbon of glutaraldehyde, so that the structure of the polyvinyl alcohol is changed. 5. In order to prevent the crosslinking effect from being influenced by the sudden polymerization phenomenon of the system, the crosslinking reaction is carried out in an acid environment, so that the reaction rate of the crosslinking reaction can be increased, and the reaction time can be shortened. 6. After the crosslinking reaction, naOH is used for neutralizing the acid remained in the crosslinking reaction, and the solution is adjusted to be neutral, so that the current safe use is facilitated; and a small amount of formaldehyde is added, so that the formaldehyde has an aldehyde group with a crosslinking function and can be used for disinfection and sterilization. 7. The fluid loss agent has good compatibility with calcium chloride and good rheological property of cement paste; the early strength is high, and the compressive strength can reach more than 15MPa at 30 ℃ for 24 h.
Drawings
FIG. 1 is a scanning electron micrograph of the surface and cross section of a filter cake according to an embodiment of the present invention.
FIG. 2 is a scanning electron micrograph of the surface and cross section of a filter cake according to example two of the present invention.
FIG. 3 is a scanning electron micrograph of the surface and cross section of a filter cake according to example three of the present invention.
FIG. 4 is a graph of water loss for API water loss measurements for examples one through three of the present invention and comparative examples.
FIG. 5 is a graph showing the water loss of the cement slurry for well cementation according to the third embodiment of the present invention.
FIG. 6 is a graph of the densification process at 60 ℃ for an embodiment of the present invention.
Fig. 7 is a water loss test result chart of the delayed slurry preparation after water distribution of the fluid loss agent according to the third embodiment of the invention.
Detailed Description
The invention relates to a well cementation method of a low-temperature shallow well, which sequentially comprises the following steps: the method comprises the steps of running a casing string in a well after the well is communicated, wherein floating shoes are arranged at the bottoms of the casing string, floating hoops are arranged above the floating shoes at intervals of one casing, a joint top section is arranged at the top of the casing string, and drilling fluid is filled in each casing after each casing is run into the well; secondly, a cementing head is installed on the jacking joint, a rubber plug is arranged in the upper part of the cementing head, and the bottom of the rubber plug abuts against a rubber plug stop pin; the top of the cement head is provided with a plug pressing liquid inlet, and the side wall of the middle part of the cement head is symmetrically provided with a low-temperature well cementation cement slurry inlet and a drilling fluid inlet; thirdly, the mud pump is started to send the drilling fluid into the inner cavity of the casing, the drilling fluid enters the borehole annulus from the floating shoe at the bottom of the casing, flows back to the ground along the borehole annulus upwards, and the rock debris in the borehole is cleaned to the ground; fourthly, injecting the prepared isolation liquid into the sleeve string by using a cement truck; fifthly, injecting the prepared low-temperature well cementation cement slurry into the casing string by using a cement truck until the low-temperature well cementation cement slurry reaches the designed well cementation amount; sixthly, removing a rubber plug stop pin on the cement head, releasing the rubber plug, injecting plugging liquid into the cement vehicle through a plugging liquid inlet, and pushing the rubber plug to move downwards by the plugging liquid; starting a mud pump, injecting drilling fluid to replace slurry, pushing the plugging fluid to move downwards, pushing the low-temperature well cementation cement slurry to move downwards through a rubber plug, pushing the spacer fluid to move upwards after the low-temperature well cementation cement slurry enters a borehole annulus from a floating shoe, and pushing the drilling fluid to move upwards through the spacer fluid; and when the rubber plug moves downwards to the flow blocking plate of the float collar, collision pressure is generated, the slurry pump is immediately turned off, and at the moment, the low-temperature well cementation cement slurry returns to the preset well section and enters the waiting setting.
Example one
The isolation liquid in step four of the invention comprises the following raw material components in parts by weight: 400 parts of suspending agent TAS155:2 parts of surfactant XP-1:4 parts of an anti-collapse release agent JS-1:12 parts of barite powder: 180 parts. The preparation method of the anti-collapse separant JS-1 sequentially comprises the following steps: the method comprises the steps of heating 100 parts of deionized water to 70 ℃, adding 4 parts of octylphenol polyoxyethylene ether, cooling to 60 ℃, adding 18 parts of vinyl triethoxysilane, preserving heat, stirring for 2 hours, stirring at 300rpm for 20 minutes, stirring at 300rpm for 30 minutes, and stirring at 150rpm for the rest of time to obtain silicone pre-polymerization emulsion; dissolving 2 parts of sodium dodecyl benzene sulfonate in 100 parts of deionized water, and then dropwise adding an acrylic acid-acetic monomer, wherein the acrylic acid-acetic monomer is premixed with 9 parts of methyl methacrylate, 18 parts of butyl acrylate and 4 parts of hydroxyethyl methacrylate, and stirring for 0.5 hour at a rotating speed of more than 300rpm to obtain a pre-emulsion A; thirdly, adding 0.3 part of potassium persulfate into 100 parts of deionized water to prepare a solution B; stirring the organic silicon pre-polymerization emulsion at the rotating speed of 300rpm, heating to 70 ℃, slowly dropwise adding the pre-emulsion A and the solution B at the same time, after dropwise adding for 45 minutes, heating to 80 ℃, stirring at the rotating speed of 150rpm, keeping the temperature for 2 hours, and then cooling to 35 ℃; and fifthly, regulating the pH value to 7 by using triethanolamine to obtain the collapse preventing separant JS-1.
The preparation method of the low-temperature well cementation cement slurry in the step fifthly sequentially comprises the following steps: pouring 4.8 parts of fluid loss additive and 2.4 parts of dispersant USZ into 352 parts of deionized water and stirring uniformly; step b: mixing 800 parts of G-grade oil well cement, 16 parts of calcium chloride and 32 parts of silica fume in a dry powder manner; step c: and (c) putting the mixed dry powder in the step (b) into the solution in the step (a) and uniformly stirring to obtain the low-temperature well cementing cement slurry. The preparation method of the fluid loss agent sequentially comprises the following steps: (1) 6 parts of polyvinyl alcohol PVA1788 is dissolved in 100 parts of deionized water to prepare a polyvinyl alcohol aqueous solution; (2) adding 10 parts of cross-linking agent glutaraldehyde into polyvinyl alcohol aqueous solution, stirring for 20 minutes, and heating to 50 ℃ while stirring; (3) adjusting the pH value to 4 by using 37 percent concentrated salt, continuously stirring and reacting for 1 hour, and carrying out chemical reaction under an acidic condition; (4) and (3) adjusting the pH value to 7 by using a NaOH solution, cooling to room temperature, adding 1 part of formaldehyde solution, and uniformly mixing to obtain the fluid loss agent.
Example two
According to the invention, the isolation liquid comprises the following raw material components in parts by weight: 400 parts of suspending agent TAS155:2 parts of surfactant XP-1:4 parts of an anti-collapse separant JS-1:16 parts of barite powder: 300 parts. The preparation method of the anti-collapse release agent JS-1 sequentially comprises the following steps: the preparation method comprises the steps of heating 100 parts of deionized water to 70 ℃, adding 4 parts of octylphenol polyoxyethylene ether, cooling to 60 ℃, adding 20 parts of vinyl triethoxysilane, preserving heat, stirring for 2 hours, stirring for 20 minutes at a rotating speed of 400rpm, stirring for 30 minutes at a rotating speed of 300rpm, and stirring for 180rpm in the rest of time to obtain silicone pre-polymerization emulsion; dissolving 2 parts of sodium dodecyl benzene sulfonate in 100 parts of deionized water, and then dropwise adding an acrylic acid-acetic monomer, wherein the acrylic acid-acetic monomer is premixed with 10 parts of methyl methacrylate, 20 parts of butyl acrylate and 4 parts of hydroxyethyl methacrylate, and stirring at the rotating speed of 320rpm for 0.5 hour to obtain a pre-emulsion A; thirdly, adding 0.4 part of potassium persulfate into 100 parts of deionized water to prepare a solution B; stirring the organic silicon pre-polymerization emulsion at the rotating speed of 300rpm, heating to 70 ℃, slowly dropwise adding the pre-emulsion A and the solution B at the same time, after dropwise adding is completed within 50 minutes, heating to 80 ℃, stirring at the rotating speed of 180rpm, keeping the temperature for 2 hours, and then cooling to 40 ℃; and fifthly, regulating the pH value to 7.5 by using triethanolamine to obtain the collapse preventing separant JS-1.
The preparation method of the low-temperature well cementation cement slurry in the step fifthly sequentially comprises the following steps: 8 parts of fluid loss additive and 2.4 parts of dispersant USZ are poured into 352 parts of deionized water and stirred uniformly; step b: mixing 800 parts of G-grade oil well cement, 20 parts of calcium chloride and 36 parts of micro silicon powder in a dry powder manner; step c: and (c) putting the mixed dry powder in the step (b) into the solution in the step (a) and uniformly stirring to obtain the low-temperature well cementing cement slurry. The preparation method of the fluid loss agent sequentially comprises the following steps: (1) dissolving 7 parts of polyvinyl alcohol PVA1788 in 100 parts of deionized water to prepare a polyvinyl alcohol aqueous solution; (2) adding 11 parts of cross-linking agent glutaraldehyde into a polyvinyl alcohol aqueous solution, stirring for 25 minutes, and heating to 55 ℃ while stirring; (3) adjusting the pH value to 4.5 by using 37 percent concentrated salt city, continuously stirring for reaction for 1 hour, and carrying out chemical reaction under an acidic condition; (4) and adjusting the pH value to 7.5 by using a NaOH solution, cooling to room temperature, adding 1.2 parts of formaldehyde solution, and uniformly mixing to obtain the fluid loss agent.
EXAMPLE III
According to the invention, the isolation liquid comprises the following raw material components in parts by weight: 400 parts of suspending agent TAS155:2 parts of surfactant XP-1:4 parts of an anti-collapse release agent JS-1:20 parts of barite powder: 490 parts. The preparation method of the anti-collapse separant JS-1 sequentially comprises the following steps: firstly, heating 100 parts of deionized water to 70 ℃, adding 4 parts of octylphenol polyoxyethylene ether, cooling to 60 ℃, adding 22 parts of vinyl triethoxysilane, preserving heat, stirring for 2 hours, stirring at a rotating speed of 500rpm for 20 minutes, then at a rotating speed of 300rpm for 30 minutes, and stirring at a rotating speed of 200rpm for the rest of time to obtain silicone pre-polymerization emulsion; dissolving 2 parts of sodium dodecyl benzene sulfonate in 100 parts of deionized water, and then dropwise adding an acrylic acid-acetic monomer, wherein the acrylic acid-acetic monomer is premixed with 11 parts of methyl methacrylate, 22 parts of butyl acrylate and 4 parts of hydroxyethyl methacrylate, and stirring at the rotating speed of 350rpm for 0.5 hour to obtain a pre-emulsion A; thirdly, adding 0.5 part of potassium persulfate into 100 parts of deionized water to prepare a solution B; stirring the organic silicon pre-polymerization emulsion at the rotating speed of 300rpm, heating to 70 ℃, slowly dropwise adding the pre-emulsion A and the solution B at the same time, after dropwise adding for 1 hour, heating to 80 ℃, stirring at the rotating speed of 200rpm, keeping the temperature for 2 hours, and then cooling to 40 ℃; and fifthly, regulating the pH value to 8 by using triethanolamine to obtain the collapse preventing separant JS-1.
The preparation method of the low-temperature well cementation cement slurry in the step fifthly sequentially comprises the following steps: pouring 12 parts of fluid loss additive and 2.4 parts of dispersant USZ into 352 parts of deionized water and stirring uniformly; step b: mixing 800 parts of G-grade oil well cement, 24 parts of calcium chloride and 40 parts of silica fume in a dry powder manner; step c: and (c) putting the mixed dry powder in the step (b) into the solution in the step (a) and uniformly stirring to obtain the low-temperature well cementing cement slurry. The preparation method of the fluid loss agent sequentially comprises the following steps: (1) 8 parts of polyvinyl alcohol PVA1788 is dissolved in 100 parts of deionized water to prepare a polyvinyl alcohol aqueous solution; (2) adding 13 parts of cross-linking agent glutaraldehyde into the polyvinyl alcohol aqueous solution, stirring for 30 minutes, and heating to 60 ℃ while stirring; (3) adjusting the pH value to 5 by using 37 percent concentrated salt, continuously stirring for reaction for 1 hour, and carrying out chemical reaction under an acidic condition; (4) and adjusting the pH value to 8 by using a NaOH solution, cooling to room temperature, adding 1.5 parts of formaldehyde solution, and uniformly mixing to obtain the fluid loss agent.
1. And (3) filtering the spacer fluid in the first to third embodiments under medium pressure to obtain a filter cake, standing the filter cake at 30 ℃ for one day, and then performing scanning electron microscope analysis, wherein the scanning electron microscope pictures of the surface and the section of the filter cake are shown in figures 1 to 3.
As is clear from fig. 1 to 3, the cake surface had a clear milky white film. As can be seen from the comparison of FIGS. 1 to 3, the coverage area of the membrane varies with the addition of the anti-collapse release agent JS-1, regardless of the surface or cross section of the filter cake. When 16 parts of the anti-collapse release agent JS-1 is added, the surface of the filter cake is basically and uniformly covered with a layer of film. When the addition of the anti-collapse release agent JS-1 is increased to 20 parts, the film covering the surface and the cross section of the filter cake is not obviously changed, so the formula of the second embodiment is most economical, and the anti-collapse performance is also good.
2. The rheological properties of the spacers of different densities of the first to the third examples were tested at normal temperature and 60 ℃, and the test results are shown in table 1:
wherein, n: prevalence index, K: consistency factor, η p: plastic viscosity,. Tau.o: dynamic shear stress. It can be seen that the viscosity and shear force of the spacer fluid increase with increasing density; the plastic viscosity and dynamic shear stress of the same composition of spacer fluid increase with increasing temperature. The rheological curve of the spacer fluid is more regular under the condition of 60 ℃, the change of the n value is always in the range of 0.6-0.7, and the spacer fluid has good rheological property and mud cake carrying performance in the range. Compared with the common spacer fluid, the popularity index is less than that of the common formula, and the spacer fluid has good advantages in rheology and mud cake carrying.
3. And (3) inspecting the suspension stability of the isolation liquid with different densities: the spacers of examples one to three were placed in a water bath at room temperature and 60 ℃ for 8 hours, and then the density of the solutions was measured at three different positions, i.e., the middle and lower parts, and the results are shown in table 2:
from the above table, it can be seen that the density difference of the upper, middle and lower parts of each group of the isolation liquid after standing for 8 hours is smaller no matter at normal temperature or at 60 ℃, but the isolation liquid can meet the construction requirements; compared with the common spacer fluid in the current market, has obvious advantages.
4. And (3) inspecting the API water loss of the spacer fluid with different densities: the requirement for the water loss of the spacer fluid is that the water loss is generally less than 150 mL/(30 min, 7 MPa). The low water loss has certain significance for controlling the collapse of the well wall and reducing the damage of the stratum, can keep the performance of the spacer fluid unchanged, and can better play a role in well cementation construction.
The test results of the API water loss test on the spacers of the first to third examples are shown in table 3, and it can be seen that the water loss is much lower than 150 mL/(30 min, 7 MPa):
the water loss curve was plotted for the test procedure at room temperature, as shown in fig. 4, and it can be seen that: along with the increase of the density of the isolation liquid, the API water loss amount of the isolation liquid is gradually reduced, the rapid increase of the water loss amount is concentrated within 5 minutes, the increase of the water loss amount is obviously slowed after 5 minutes, and compared with the conventional isolation liquid, the isolation liquid can rapidly control the water loss in a low-temperature environment, and is favorable for protecting the stability of a well wall.
5. Carrying out a washing efficiency evaluation experiment on the isolation solution of the second embodiment; firstly weighing the outer cylinder of the rheometer, wherein the weight is 153.83g, then soaking the outer cylinder of the rheometer in the oil-based drilling fluid for 2min, taking out the outer cylinder and weighing when mud does not drip to obtain 161.66g, then flushing the outer cylinder on the rheometer for 10 min by using the spacer fluid of the second embodiment at the rotating speed of 300rpm, taking out the outer cylinder, weighing when no liquid drips, wherein the weight is 154.06g, and the flushing efficiency is calculated as follows: (161.66-154.06)/(161.66-153.83) × 100% ≈ 97.1%. The flushing efficiency of the spacer fluid on the oil-based drilling fluid reaches more than 80 percent, namely the spacer fluid is qualified, and the flushing efficiency of the spacer fluid is far higher than that of a conventional product.
6. The compatibility of the spacer fluid and the polysulfonate drilling fluid is inspected: the spacer fluid and the polysulfonate drilling fluid of the second embodiment are sequentially mixed according to the proportion and sequence in the following table, and are fully stirred and mixed on a high-speed stirrer, and then the spacer fluid and the polysulfonate drilling fluid are transferred to a flow rate rotational viscometer to measure the rheological property, and the data of the test results are shown in table 4:
it can be seen from table 4 that the addition of the spacer fluid makes the dynamic shear stress τ o of the drilling fluid smaller, and the dynamic shear stress τ o is smaller than that of the drilling fluid raw stock after being mixed in any proportion, which shows that the spacer fluid of the present invention not only can not increase the dynamic shear stress value of the drilling fluid, but also has the function of reducing the dynamic shear force of the drilling fluid, and the spacer fluid is positioned before the low-temperature well cementation cement slurry in the displacement process, and is in direct contact with the drilling fluid, so that the shear force of the displaced drilling fluid can be reduced, the flowing resistance is reduced, and the displacement of the drilling fluid is facilitated.
In the invention, the suspending agent TAS155 adopts the product of Tianjin BaoEn petroleum engineering technology Limited company, and the execution standard is as follows: Q/SH1025-0861. The surfactant XP-1 adopts a product of Weihui chemical company Limited and implements the standard: Q/SHCG-32. The barite powder is prepared from the product of Xinzheng Meijiu industry Co., ltd, zhengzhou city, and meets GB/T5005-1994 standard.
The products of Shanghai national medicine group chemical reagent company Limited can be adopted as the octyl phenol polyoxyethylene ether OP-10, the vinyl triethoxysilane VETS, the sodium dodecyl benzene sulfonate SDBS, the potassium persulfate KPS, the triethanolamine TEA, the methyl methacrylate MMA, the butyl acrylate BA and the hydroxyethyl methacrylate HEMA.
7. The API water loss of the medium and low temperature well cementation cement slurry in the first to third examples at 25 ℃ and 60 ℃ is respectively tested, the total test time is 30 minutes, and the test results are shown in Table 5:
the water loss is lower than 90 mL/(30 min, 7 MPa), and is far lower than the requirement that the water loss of the low-temperature well cementation cement slurry is lower than 150 mL/(30 min, 7 MPa).
8. The water loss rate of the low-temperature well cementation cement slurry is examined: the total water loss of the low temperature cementing slurry of example three was 32mL at 60 ℃ for 30 minutes, and the water loss process was recorded for the first 3 minutes, as shown in fig. 5. It can be found that the water loss is rapidly increased to 24mL within 14s, the test time is continuously prolonged, the water loss is slowly increased, and the water loss is 26mL after 3 minutes, which shows that most of the water loss of the cement paste occurs at the initial stage, and exceeds 30 seconds, and the water loss speed of the cement paste is very slow. The shorter the cement slurry is controlled to lose water, the damage of the water loss to the stratum can be reduced, the safety of the well wall can be protected, and well cementation safety accidents caused by the instability of the well wall due to the water loss of the cement slurry can be prevented.
9. The test examples one to three, the thickening times of the low temperature cementing slurry at 30 ℃ and 60 ℃, the test results are shown in table 6:
the experimental results show that under the low-temperature environment of 30 ℃ and 60 ℃, the thickening time of the low-temperature well cementation cement slurry is 30 minutes to 60 minutes more than that of the low-temperature well cementation cement slurry from the underground injection to the completion of grouting, and the construction requirements can be completely met.
The thickening process at 60 ℃ in the first embodiment is shown in fig. 6, and it can be seen that the thickening curve of the low-temperature well cementation cement slurry has good linearity, the curve is in a 'right-angle' shape, the inflection point is obvious, the 'bulge' phenomenon that the consistency slowly rises is avoided, the consistency before the inflection point is basically stable, the consistency rapidly rises after the inflection point is reached, and the construction requirement of well cementation is completely met.
10. The compressive strength of the medium-low temperature well cementation cement slurry in the first to the third test examples at 30 ℃ and 60 ℃ is shown in the following table 7:
as can be seen from Table 7, the low-temperature well cementation cement slurry has short waiting time under a low-temperature environment, and the compressive strength is more than 15MPa after 24 hours; after 48 hours, the compressive strength is more than 22MPa, and the strength is developed well. Generally, for a low-temperature well, the compressive strength after 24 hours is more than 7MPa, and the low-temperature well cementing cement paste is qualified, and the compressive strength index of the low-temperature well cementing cement paste is far higher than that of the conventional low-temperature well cementing cement paste.
11. Investigating the influence of the standing time on the effect of the fluid loss agent: after the fluid loss agent is distributed with water, the fluid loss agent is placed for 1 to 35 days, the fluid loss agent taken and placed every five days is subjected to slurry distribution, the cement slurry formula of the third embodiment is adopted, the API fluid loss test at 60 ℃ is carried out after slurry distribution, the test time is 30 minutes each time, the pressure is 7MPa, the longest placing time is 35 days, and the test result is shown in figure 7. As can be seen from FIG. 7, the water loss of the cement paste is slightly increased along with the gradual extension of the placing time, but the cement paste has small fluctuation and stable performance, can meet the well cementation delay period of most well sites, avoids the waste of abandoning and saves the production cost.
Claims (8)
1. A well cementation method of a low-temperature shallow well is characterized by sequentially comprising the following steps: the method comprises the steps of running a casing string in a well after the well is communicated, wherein floating shoes are arranged at the bottoms of the casing string, floating hoops are arranged above the floating shoes at intervals of one casing, a joint top section is arranged at the top of the casing string, and drilling fluid is filled in each casing after each casing is run into the well; secondly, a cementing head is installed on the jacking joint, a rubber plug is arranged in the upper part of the cementing head, and the bottom of the rubber plug abuts against a rubber plug stop pin; the top of the cement head is provided with a plug pressing liquid inlet, and the side wall of the middle part of the cement head is symmetrically provided with a low-temperature well cementation cement slurry inlet and a drilling liquid inlet; thirdly, the mud pump is started to send the drilling fluid into the inner cavity of the casing, the drilling fluid enters the borehole annulus from the floating shoe at the bottom of the casing, flows back to the ground along the borehole annulus upwards, and the rock debris in the borehole is cleaned to the ground; fourthly, injecting the prepared isolation liquid into the sleeve string by using a cement truck; fifthly, injecting the prepared low-temperature well cementation cement slurry into the casing string by using a cement truck until the low-temperature well cementation cement slurry reaches the designed well cementation amount; sixthly, removing a rubber plug stop pin on the cement head, releasing the rubber plug, injecting plugging liquid into the cement vehicle through a plugging liquid inlet, and pushing the rubber plug to move downwards by the plugging liquid; starting a mud pump, injecting drilling fluid to replace slurry, pushing the plugging fluid to move downwards, pushing the low-temperature well cementation cement slurry to move downwards through a rubber plug, pushing the spacer fluid to move upwards after the low-temperature well cementation cement slurry enters a borehole annulus from a floating shoe, and pushing the drilling fluid to move upwards through the spacer fluid; when the rubber plug moves downwards to the flow blocking plate of the float collar, collision pressure is generated, the slurry pump is immediately turned off, and at the moment, the low-temperature well cementation cement slurry returns to the preset well section and enters the waiting setting;
the isolation liquid in the fourth step comprises the following raw material components in parts by weight: 400 parts of suspending agent TAS155:2 parts of surfactant XP-1:4 parts of an anti-collapse release agent JS-1:12-20 parts of barite powder: 180-490 parts;
the preparation method of the anti-collapse release agent JS-1 sequentially comprises the following steps: firstly, heating 100 parts of deionized water to 70 ℃, adding 4 parts of octylphenol polyoxyethylene ether, cooling to 60 ℃, adding 18-22 parts of vinyl triethoxysilane, preserving heat, stirring for 2 hours, stirring for 20 minutes at a rotating speed of 300-500rpm, stirring for 30 minutes at a rotating speed of 300rpm, and stirring for 150-200rpm at the rest of time to obtain silicone pre-polymerization emulsion; dissolving 2 parts of sodium dodecyl benzene sulfonate in 100 parts of deionized water, then dropwise adding an acrylic acid-acetic monomer, wherein the acrylic acid-acetic monomer is premixed with 9-11 parts of methyl methacrylate, 18-22 parts of butyl acrylate and 4 parts of hydroxyethyl methacrylate, and stirring for 0.5 hour at a rotating speed of more than 300rpm to obtain a pre-emulsion A; thirdly, adding 0.3-0.5 part of potassium persulfate into 100 parts of deionized water to prepare a solution B; stirring the organic silicon pre-polymerization emulsion at the rotating speed of 300rpm, heating to 70 ℃, slowly dropwise adding the pre-emulsion A and the solution B, finishing dropwise adding within 1 hour, heating to 80 ℃, stirring at the rotating speed of 150-200rpm, keeping the temperature for 2 hours, and cooling to below 40 ℃; fifthly, regulating the pH value to 7-8 by using triethanolamine to obtain the anti-collapse separant JS-1;
step fifthly, the low-temperature well cementing cement slurry comprises the following raw material components in parts by weight: 800 parts of fluid loss agent: 4.8-12 parts of calcium chloride: 16-24 parts of micro silicon powder: 32-40 parts of dispersant USZ:2.4 parts and deionized water: 352 parts of a binder; the fluid loss agent comprises the following raw material components in parts by weight: 100 parts of polyvinyl alcohol PVA1788:6-8 parts of cross-linking agent glutaraldehyde: 10-13 parts and formaldehyde: 1-1.5 parts.
2. The method for cementing a shallow well at low temperature according to claim 1, wherein the spacer fluid comprises the following raw material components by weight: 400 parts of suspending agent TAS155:2 parts of surfactant XP-1:4 parts of an anti-collapse release agent JS-1:12 parts of barite powder: 180 parts of (A); the anti-collapse release agent JS-1 comprises the following raw material components in percentage by weight, and deionized water: 300 parts of octyl phenol polyoxyethylene ether: 4 parts of vinyltriethoxysilane: 18 parts of sodium dodecyl benzene sulfonate: 2 parts of methyl methacrylate: 9 parts of butyl acrylate: 18 parts of hydroxyethyl methacrylate: 4 parts and potassium persulfate: 0.3 part.
3. The method for cementing a shallow well at low temperature according to claim 1, wherein the raw material components and weight contents of the spacer fluid are as follows: 400 parts of suspending agent TAS155:2 parts of surfactant XP-1:4 parts of an anti-collapse release agent JS-1:16 parts of barite powder: 300 parts of (A); the anti-collapse release agent JS-1 comprises the following raw material components and weight content, deionized water: 300 parts of octyl phenol polyoxyethylene ether: 4 parts of vinyltriethoxysilane: 20 parts of sodium dodecyl benzene sulfonate: 2 parts of methyl methacrylate: 10 parts of butyl acrylate: 20 parts of hydroxyethyl methacrylate: 4 parts and potassium persulfate: 0.4 part.
4. The method for cementing a shallow well at low temperature according to claim 1, wherein the spacer fluid comprises the following raw material components by weight: 400 parts of suspending agent TAS155:2 parts of surfactant XP-1:4 parts of an anti-collapse release agent JS-1:20 parts of barite powder: 490 parts; the anti-collapse release agent JS-1 comprises the following raw material components in percentage by weight, and deionized water: 300 parts of octyl phenol polyoxyethylene ether: 4 parts of vinyltriethoxysilane: 22 parts of sodium dodecyl benzene sulfonate: 2 parts of methyl methacrylate: 11 parts and butyl acrylate: 22 parts of hydroxyethyl methacrylate: 4 parts and potassium persulfate: 0.5 part.
5. The method for cementing a shallow well at low temperature according to any one of claims 1 to 4, wherein the preparation of the cement slurry for cementing at low temperature mentioned in the step fifthly comprises the following steps in sequence, namely step a: pouring the fluid loss agent and the dispersing agent USZ into deionized water and stirring uniformly; step b: mixing dry powder of G-grade oil well cement, calcium chloride and micro silicon powder; step c: b, putting the mixed dry powder in the step a into the solution in the step a, and uniformly stirring to obtain low-temperature well cementing cement slurry; the preparation method of the fluid loss agent sequentially comprises the following steps: (1) dissolving polyvinyl alcohol PVA1788 in deionized water to prepare a polyvinyl alcohol aqueous solution; (2) adding cross-linking agent glutaraldehyde into polyvinyl alcohol aqueous solution, stirring for 20-30 minutes, and heating to 50-60 ℃ while stirring; (3) adjusting the pH value to 4-5 with concentrated hydrochloric acid, continuously stirring for reaction for 1 hour, and carrying out chemical reaction under an acidic condition; (4) and adjusting the pH value to 7-8 by using a NaOH solution, cooling to room temperature, adding a formaldehyde solution, and uniformly mixing to obtain the fluid loss agent.
6. The method for cementing a shallow well at low temperature according to claim 5, wherein the weight content of part of the raw materials is as follows, fluid loss agent: 4.8 parts of calcium chloride: 16 parts of micro silicon powder: 32 parts of polyvinyl alcohol PVA1788:6 parts of cross-linking agent glutaraldehyde: 10 parts of formaldehyde: 1 part.
7. The method for cementing a low-temperature shallow well according to claim 5, wherein the weight contents of part of raw materials are as follows, and the fluid loss additive is: 8 parts of calcium chloride: 20 parts of micro silicon powder: 36 parts of polyvinyl alcohol PVA1788:7 parts of cross-linking agent glutaraldehyde: 11 parts and formaldehyde: 1.2 parts.
8. The method for cementing a shallow well at low temperature according to claim 5, wherein the weight content of part of the raw materials is as follows, fluid loss agent: 12 parts of calcium chloride: 24 parts of micro silicon powder: 40 parts of polyvinyl alcohol PVA1788:8 parts of cross-linking agent glutaraldehyde: 13 parts and formaldehyde: 1.5 parts.
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