CN113438970A

CN113438970A - Crosslinking agent and preparation thereof

Info

Publication number: CN113438970A
Application number: CN202180002071.3A
Authority: CN
Inventors: 孟红卫; 冯三林; 周崇博; 张兆辉; 杨俊艳; 张余岐; 张爰辉; 张福来
Original assignee: Individual
Current assignee: Individual
Priority date: 2020-01-18
Filing date: 2021-01-18
Publication date: 2021-09-24
Also published as: AU2021208183A1; WO2021143904A1; CN111205847B; AU2020202077A1; CN111205847A

Abstract

The invention discloses a cross-linking agent and preparation thereof, wherein a preparation device comprises a reaction kettle, a filter cylinder, a stirring mechanism, a driving mechanism, a discharge pipe, a mixing spray pipe and a circulating pump, and the cross-linking agent comprises zirconium hydroxide, fatty alcohol, organic peptide chelate and polyoxyethylene laurate.

Description

Crosslinking agent and preparation thereof

Technical Field

The invention relates to a cross-linking agent and a preparation method thereof.

Background

The existing cross-linking agent needs different temperatures and pressures in different working procedures in the production process, on one hand, the difficulty of the production process is increased, and on the other hand, the requirement on the strength of equipment is high.

Disclosure of Invention

On one hand, the invention provides a preparation device of an oil well fracturing crosslinking agent, which comprises a reaction kettle separated into a first reaction cavity and a second reaction cavity by a partition plate, wherein an opening and closing filter cylinder for communicating or blocking the first reaction cavity and the second reaction cavity is constructed on the partition plate, stirring mechanisms are respectively arranged in the first reaction cavity and the second reaction cavity, a driving mechanism which is respectively in transmission connection with the two stirring mechanisms and is used for driving the stirring mechanisms to stir is installed on an end cover of the reaction kettle, a discharge pipe for communicating the first reaction cavity with the second reaction cavity is arranged at the bottom of the reaction kettle, a mixing spray pipe with one end extending into the opening and closing filter barrel is arranged on the reaction kettle, and the discharge pipe and the mixing spray pipe are respectively communicated with an inlet and an outlet of a circulating pump. .

In another aspect, the invention provides an oil well fracturing cross-linking agent for use as a cross-linking formulation for an oil field fracturing fluid, the fracturing cross-linking agent comprising zirconium hydroxide, a fatty alcohol, an organic peptide chelate, polyoxyethylene laurate, and water.

Further, the ratio of zirconium hydroxide: fatty alcohol: organic peptide chelate: lauric acid polyoxyethylene ether 25-50: 5-20: 10-33: 8-22(wt), such as zirconium hydroxide: fatty alcohol: organic peptide chelate: lauric acid polyoxyethylene ether is 30-45: 8-15: 15-28: 10-18. Preferably, the fracturing cross-linking agent comprises the following components: 38 wt% of zirconium hydroxide, 12 wt% of fatty alcohol, 23 wt% of organic peptide chelate, 14 wt% of lauric acid polyoxyethylene ether and 13 wt% of water.

Drawings

FIG. 1 is a schematic structural diagram of example 2 of the present invention;

FIG. 2 is a schematic view of the structure of FIG. 1 from another angle;

FIG. 3 is a schematic view of the structure of FIG. 1 from another angle;

FIG. 4 is a partial structural sectional view of embodiment 2 of the present invention;

fig. 5 is a schematic structural view of an on-off filter cartridge according to embodiment 2 of the present invention;

FIG. 6 is a schematic view of the structure of FIG. 5 at another angle;

FIG. 7 is a diagram illustrating a state in which the filter cartridge is opened and closed to separate the first reaction chamber and the second reaction chamber in accordance with embodiment 2 of the present invention;

FIG. 8 is a diagram illustrating a state where the filter cartridge is opened and closed to communicate the first reaction chamber and the second reaction chamber in accordance with embodiment 2 of the present invention;

FIG. 9 is a schematic structural view of a premix mechanism in embodiment 2 of the present invention;

fig. 10 is a partial structural sectional view of a premix feed mechanism according to embodiment 2 of the present invention;

FIG. 11 is a partial cross-sectional view of a mixing drum of example 2 of the present invention;

FIG. 12 is a schematic view showing the structure of a spherical filter in example 2 of the present invention;

fig. 13 is an axial structural sectional view of a spherical filter according to example 2 of the present invention.

Detailed Description

Example 1

The embodiment discloses an oil well fracturing cross-linking agent: 38 wt% of zirconium hydroxide, 12 wt% of fatty alcohol, 23 wt% of organic peptide chelate, 14 wt% of lauric acid polyoxyethylene ether and 13 wt% of water. The performance of the product was tested as follows.

Appearance of the product	Homogeneous liquid
Density (25 ℃) g/cm < 3 >	0.9-1.3
pH value (1.0% aqueous solution)	5.0-9.0
Crosslinking Properties	Good and can be hung
High heat resistance (C)	≥120

The more preferred cross-linking agent composition is: 38 wt% of zirconium hydroxide, 12 wt% of tert-butanol, peptide Asp-Glu and Ca ²⁺23 wt% of chelate, 14 wt% of lauric acid polyoxyethylene ether and 13 wt% of water.

Example 2

The embodiment discloses a preparation facilities of oil well fracturing cross-linking agent, as shown in fig. 1-4, it includes that upper end cover 10 is detachable reation kettle 1, is constructed baffle 2 in reation kettle 1, and this baffle 2 adopts the welding with reation kettle 1's fixed mode, and baffle 2 separates reation kettle 1 for first reaction chamber 3 and second reaction chamber 4. Wherein, the effect of first reaction chamber 3 and second reaction chamber 4 is used for synthesizing one dose of solution and two doses of solutions respectively, and in order to ensure at the in-process of synthesizing one dose of solution and two doses of solutions, feed liquid keeps the stirring state throughout in first reaction chamber 3 and the second reaction chamber 4, all be in the homogeneous mixing state with the feed liquid that realizes in two chambeies, be provided with rabbling mechanism respectively in first reaction chamber 3 and second reaction chamber 4, these two rabbling mechanisms are through the actuating mechanism drive of installing on reation kettle 1 end cover 10, and then stir the feed liquid in corresponding first reaction chamber 3 and the second reaction chamber 4 in step.

In the embodiment, in order to avoid increasing the investment cost of a mixing container and a stirring device while fully mixing the first solution and the second solution, as shown in fig. 4, an opening and closing filter cylinder is configured on the partition plate 2 and is used for communicating or blocking the first reaction chamber 3 and the second reaction chamber 4, so that the mixing of the first solution and the second solution can be realized, and the first solution and the second solution are gradually mixed in the continuous stirring process of the stirring mechanism.

In this embodiment, in order to make one dose of solution and two doses of solution mix under the abundant prerequisite, shorten the mix time to improve production efficiency, as shown in fig. 3, be provided with the discharging pipe 26 that both ends communicate with first reaction chamber 3 and second reaction chamber 4 respectively in reation kettle 1's below, be equipped with the compounding spray tube 9 that one end stretches into the open and close filter vat in reation kettle 1's one side, this discharging pipe 26 and compounding spray tube 9 communicate with the import and the export of a circulating pump 30 respectively. Circulating pump 30 takes out a dose solution and two doses solutions from reation kettle 1, and spray into through compounding spray tube 9 and open and close the filter vat, open and close the filter vat its interior mixed liquid and be opened and close the filter vat and filter, and enter first reaction chamber 3 and second reaction chamber 4, this part has certain pressure's mixed liquid to act on by two rabbling mechanisms stirring feed liquid, make the feed liquid in first reaction chamber 3 and the second reaction chamber 4 take place abundant disturbance, and make like this the feed liquid in reation kettle 1 send down at circulating pump 30's pump, form a lasting mixture and circulation process, and then make the mixture more abundant, and the mixing time reduces greatly, production efficiency obtains promoting by a wide margin.

As a preferred structure of the on-off filter cartridge of this embodiment, as shown in fig. 5-8, the on-off filter cartridge includes a cylinder 5 and an adjusting sleeve 6. Wherein, barrel 5 structure is in baffle 2 middle part and extends along the length direction of baffle 2, and adjusting collar 6 assembles in barrel 5, and the inner wall adaptation of adjusting collar 6 and barrel 5, and adjusting collar 6 can rotate along the axis of barrel 5 under the external force rotates. An annular mounting seat 502 is configured on the side wall of the reaction kettle 1 at one axial end of the cylinder 5, and a sealing cover 24 is detachably mounted on the mounting seat 502 through bolts and used for sealing the end of the cylinder 5. Adjusting sleeve 6 is located the one end of mount pad 502 through barrel 5 and is inserted into barrel 5, and the one end fixed mounting that is close to closing cap 24 at adjusting sleeve 6 has a handle 25, and this handle 25 has the bull stick, and the bull stick is overlapped with adjusting sleeve 6 tip fixed connection and with adjusting sleeve 6 axis, and the bull stick stretches out reation kettle 1 through closing cap 24, and the bull stick rotates with closing cap 24 and is connected. As shown in fig. 5 to 6, a plurality of communication ports 501 are opened uniformly on the circumferential surface of the cylinder 5, and each communication port 501 extends from one end of the cylinder 5 to the other end in the axial direction of the cylinder 5. The same number of screens 601 as the number of communication openings 501 is formed on the circumferential surface of the adjusting sleeve 6, which screens 601 can be adapted to the respective communication openings 501. The operator rotates the handle 25 to rotate the adjusting sleeve 6 along the axis of the barrel 5. When a dose of solution and a dose of solution are required to be prepared separately, the handle 25 is rotated until the non-filter screen 601 portion of the peripheral wall of the adjusting sleeve 6 is positioned at a position where each communication port 501 is closed, and the first reaction chamber 3 and the second reaction chamber 4 are partitioned. When a dose of solution and a dose of solution are required to be mixed, the handle 25 is rotated until the filter screen 601 and the corresponding communication port 501 are in an alignment or partially overlapping position, and the first reaction chamber 3 and the second reaction chamber 4 are communicated. In this embodiment, the filter screen 601 is disposed on the adjusting sleeve 6, so that the mixed liquid pumped into the adjusting sleeve by the circulating pump 30 is fully filtered in the process of entering the first reaction chamber 3 and the second reaction chamber 4, and thus, the purity of the finally obtained product is high. And when the outlet pressure of the circulating pump 30 is higher, the filth blockage degree of the adjusting sleeve 6 is proved to be higher, at this time, after the production is finished, the sealing cover 24 and the mounting seat 502 are disassembled, the adjusting sleeve 6 is detached from the cylinder body 5 along with the sealing cover 24, the filter screen 601 is detached from the adjusting sleeve 6, the filter screen 601 and impurities in the adjusting sleeve 6 are washed by using cleaning agents and the like, the cleaning is completed, and then the cleaning and the refilling are carried out. This embodiment is after production, need wash in reation kettle 1, and its specific washing mode is, pours into the clear water into first reaction chamber 3 and second reaction chamber 4 into, and adjustment adjusting collar 6 makes it communicate first reaction chamber 3 and second reaction chamber 4, opens circulating pump 30 and circulates, and the clear water in the reation kettle 1 of discharging after a period closes circulating pump 30, washs the end.

This embodiment is for more abundant mixed feed liquid to when saving and mixing, it can be a plurality of to open and close the cartridge filter, opens and close the cartridge filter like this and constructs on baffle 2 along the direction of height interval of baffle 2, and the quantity of compounding spray tube 9 is the same with the quantity of opening and close the cartridge filter to stretch into one by one and open and close the cartridge filter, these import of compounding spray tube 9 are parallelly connected together and communicate with circulating pump 30's export.

The mixing nozzle 9 of this embodiment is preferably configured such that, as shown in fig. 6, one end of the mixing nozzle 9 is closed and extends into the adjusting sleeve 6 along the axis of the adjusting sleeve 6, and a plurality of nozzle 901 sets are spaced along the axial direction of the mixing nozzle 9 on a part of the surface of the mixing nozzle 9 extending into the adjusting sleeve 6, each nozzle 901 set includes a plurality of nozzles 901, and the nozzles 901 are spaced along the circumferential direction of the mixing nozzle 9. Therefore, the feed liquid in the range covered by the filter screen 601 in the reaction kettle 1 is fully disturbed, and the feed liquid is fully mixed by being matched with the stirring of the stirring mechanism.

As a preferred structure of the driving mechanism and the stirring mechanism of the present embodiment, as shown in fig. 4, the stirring mechanism includes a stirring shaft 7 extending from an end cap 10 of the reaction vessel 1 into the reaction vessel 1 in a vertical direction, the stirring shaft 7 is rotatably connected to the end cap 10 of the reaction vessel 1, and a stirring blade 8 is configured on the stirring shaft 7. As shown in fig. 1, the driving mechanism includes a driving motor 11, a driving gear 13 and two driven gears 14, the driving motor 11 is assembled at the upper end of the reaction kettle 1 through a support frame 12 installed on the end cover 10, the driving gear 13 is coaxially assembled with the output shaft of the driving motor 11, the two driven gears 14 are respectively coaxially assembled on the corresponding stirring shafts 7, and the two driven gears 14 are respectively engaged with the driving gear 13. The driving motor 11 is started to drive the driving gear 13 to rotate, the driving gear 13 drives the two driven gears 14 to rotate, and then the stirring shaft 7 rotates to realize a stirring function. The driving gear 13 of the present embodiment is larger in size than the driven gear 14, and has a large transmission ratio.

In this embodiment, when one solution and two solutions are mixed, and the pre-mixing is performed during the pumping process of the circulation pump 30, so as to facilitate the subsequent mixing, as shown in fig. 3, a pre-mixing mechanism 29 is installed at the inlet end of the circulation pump 30 or the outlet end of the circulation pump 30. The pre-mixing mechanism 29 is specifically configured to include a mixing housing and a mixing drum 2906, as shown in fig. 9-11. Wherein, the mixing shell comprises an upper half shell 2902 and a lower half shell 2901 which are buckled with each other and fastened into a closed shell through bolts, the shell is a hollow cylindrical structure, a liquid inlet connector 2903 connected with an inlet pipe 27 and a liquid outlet connector 2904 communicated with an inlet of a circulating pump 30 are constructed on the upper half shell 2902, and an inlet control valve 28 is installed on the inlet pipe 27. An outlet of the circulating pump 30 is connected with an outlet pipe 31, the outlet pipe 31 is communicated with a bidirectional pipe 32, two ends of the bidirectional pipe 32 are respectively connected with the mixing spray pipe 9 and the spherical filter 3636, the two-way pipe 32 is respectively provided with a mixing control valve 33 and a discharging control valve 34, and the mixing control valve 33 and the discharging control valve 34 are respectively used for controlling the communication of the outlet pipe 31 with the mixing spray pipe 9 and the spherical filter 36. A base 2905 is mounted to a lower portion of the lower housing half 2901. The mixing drum 2906 is a hollow cylindrical structure, the mixing drum 2906 is assembled in the mixing housing, the axes of the mixing drum and the mixing housing are coincident, and the axial two ends of the mixing drum 2906 are rotatably connected with the mixing drum 2906 through rotating shafts. Mixing blades 2907 are uniformly configured on the circumferential surface of the mixing drum 2906, each mixing blade 2907 extends from one end to the other end of the mixing drum 2906 along the axial direction of the mixing drum 2906, and the mixing drum 2906 continuously impacts the mixing blades 2907 to rotate through the feed liquid with pressure entering the mixing housing, so that the pumped feed liquid of the first reaction chamber 3 and the pumped feed liquid of the second reaction chamber 4 are premixed.

In this embodiment, in order to filter impurities in the final product, as shown in fig. 1, a spherical filter 36 is installed on the discharge pipe of the reaction kettle 1. The spherical filter 36 specifically includes a spherical housing and a hollow spherical filter element 3605, as shown in fig. 12 and 13. The spherical shell comprises a first hemispherical shell 3601 and a second hemispherical shell 3602 which are mutually buckled, and a filter inlet joint 3603 and a filter outlet joint 3604 are respectively constructed on the first hemispherical shell 3601 and the second hemispherical shell 3602. The spherical filter element 3605 is assembled in the spherical shell and provided with an opening for liquid to enter, a recoil valve 3606 is fixedly connected to the spherical filter element 3605, one end of a valve rod of the recoil valve 3606 is fixedly connected with the spherical filter element 3605, and the other end of the valve rod extends outwards along the radial direction of the spherical filter element 3605 to form the spherical shell and is rotatably connected with the spherical shell. When ball filter 36 is in normal operation, the opening is aligned with filter inlet fitting 3603; when it is desired to backflush the spherical filter element 3605, the backflush valve 3606 is operated to rotate to align the opening with the filter outlet fitting 3604, and then the liquid passing through the spherical filter 36 from the filter inlet fitting 3603 flushes the impurities from the spherical filter element 3605 clean. And in order to identify which station the recoil valve 3606 is at, a pointer 3607 is fixed on a valve rod of the recoil valve 3606.

Example 3

A preparation method of a fracturing cross-linking agent comprises the following steps:

s1, injecting water into the corresponding first reaction cavity 3 and the second reaction cavity 4 through the first water inlet pipe 37 and the second water inlet pipe 38 respectively;

s2, starting the driving motor 11 to enable the two stirring mechanisms to stir the water in the first reaction chamber 3 and the water in the second reaction chamber 4 respectively;

s3, adding zirconium hydroxide into a first reaction chamber 3 through a branch pipe A17 and a first adapter pipe 16 and a first feeding main pipe 15 which are sequentially communicated with the zirconium hydroxide, and adding the organic peptide chelate into a second reaction chamber 4 through a branch pipe D22 and a second adapter pipe 21 and a second feeding main pipe 20 which are sequentially communicated with the organic peptide chelate;

s4, after 30min, adding fatty alcohol into the first reaction chamber 3 through a branch pipe B18 and a first adapter pipe 16 and a first feeding main pipe 15 which are sequentially communicated with the fatty alcohol, and after 40min, adding lauric acid polyoxyethylene ether into the second reaction chamber 4 through a branch pipe E23 and a second adapter pipe 21 and a second feeding main pipe 20 which are sequentially communicated with the lauric acid polyoxyethylene ether;

s5, after 40min, adding fatty alcohol into the first reaction chamber 3 through a branch pipe C19 and a first adapter pipe 16 and a first feeding main pipe 15 which are sequentially communicated with the branch pipe C19;

s6, after 40min, rotating the handle 25 to align the filter screen 601 of the adjusting sleeve 6 with the communication port 501 on the cylinder 5 so as to ensure that the first reaction chamber 3 is communicated with the second reaction chamber 4;

s7, starting a circulating pump 30, and pumping feed liquid in the first reaction cavity 3 and the second reaction cavity 4 into an adjusting sleeve 6 through the circulating pump 30 through a mixing spray pipe 9;

s8, stopping the stirring mechanism and the circulating pump 30 after 50 min;

s9, after the material liquid in the reaction kettle 1 is stable, closing the control valve on the mixing spray pipe 9, opening the control valve on the discharging pipe 35, then opening the circulating pump 30, and pumping the finished material liquid in the reaction kettle 1 into the collecting container through the discharging pipe 35 by the circulating pump 30.

Claims

The device for preparing the oil well fracturing cross-linking agent comprises a reaction kettle which is separated into a first reaction cavity and a second reaction cavity through a partition plate, wherein an opening and closing filter cylinder which is used for communicating or blocking the first reaction cavity and the second reaction cavity is constructed on the partition plate, stirring mechanisms are respectively arranged in the first reaction cavity and the second reaction cavity, a driving mechanism which is respectively in transmission connection with the two stirring mechanisms and used for driving the stirring mechanisms to stir is installed on an end cover of the reaction kettle, a discharge pipe which is communicated with the first reaction cavity and the second reaction cavity is arranged at the bottom of the reaction kettle, one end of the discharge pipe which is arranged on the reaction kettle stretches into a mixing spray pipe which is used for opening and closing the filter barrel, and the discharge pipe and the mixing spray pipe are respectively communicated with an inlet and an outlet of a circulating pump.
The apparatus of claim 1, wherein: the on-off filter cartridge includes the structure in the baffle middle part and the barrel that extends along the length direction of baffle, in the barrel is equipped with the axis pivoted adjusting collar that can follow the barrel in, the adjusting collar rotates through the handle rather than linking firmly, just the handle with reation kettle's lateral wall rotates to be connected, and it has a plurality of intercommunication mouths to open at the interval on the global of barrel, in it has a plurality of filter screens to construct on the global of adjusting collar, works as when the filter screen aligns or partially overlaps with corresponding intercommunication mouth, first reaction chamber and second reaction chamber are linked together, works as when the non-filter screen part of perisporium of adjusting collar seals each intercommunication mouth, first reaction chamber and second reaction chamber are cut off.
The apparatus of claim 1, wherein: one end of the mixing spray pipe is closed, the end extends into the adjusting sleeve along the axis of the adjusting sleeve, and a plurality of nozzles are arranged at intervals along the axial direction of the part of the mixing spray pipe extending into the adjusting sleeve.
The apparatus of claim 1, wherein: the driving mechanism comprises a driving motor arranged at the top end of the reaction kettle, a driving gear is arranged on an output shaft of the driving motor, driven gears are respectively arranged on two stirring shafts of the two stirring mechanisms, and the two driven gears are respectively meshed with the driving gear.
The apparatus of claim 1, wherein: and a premix mechanism is arranged at the inlet end of the circulating pump and/or the outlet end of the circulating pump.
The apparatus of claim 1, wherein: the premixing mechanism comprises a detachable mixing shell, a mixing rotary drum which is rotatably connected with the mixing shell is assembled in the mixing shell, mixing blades are uniformly constructed on the circumferential surface of the mixing rotary drum, each mixing blade extends from one end of the mixing rotary drum to the other end along the axial direction of the mixing rotary drum, and the mixing rotary drum continuously impacts the mixing blades to rotate through a feed liquid with pressure entering the mixing shell so as to form premixing of the feed liquid of the first reaction cavity and the feed liquid of the second reaction cavity.
The apparatus of claim 1, wherein: the reaction kettle is characterized in that a spherical filter is arranged on a discharging pipe of the reaction kettle and comprises a detachable spherical shell and a spherical filter element assembled in the spherical shell, and the spherical filter element is fixedly connected to a recoil valve rotatably connected with the spherical shell.
The apparatus of claim 7, wherein: the spherical filter element is hollow.
A method of preparing a fracture cross-linking agent using the apparatus of any preceding claim, the method comprising the steps of:

s1, respectively injecting water into the first reaction cavity and the second reaction cavity;

s2, starting a driving motor to enable the two stirring mechanisms to stir the water in the first reaction cavity and the water in the second reaction cavity respectively;

s3, adding zirconium hydroxide into the first reaction cavity, and adding the organic peptide chelate into the second reaction cavity;

s4, after 30min, adding fatty alcohol into the first reaction cavity, and after 40min, adding lauric acid polyoxyethylene ether into the second reaction cavity;

s5, after 40min, adding fatty alcohol into the first reaction cavity;

s6, after 40min, rotating the handle to align the filter screen of the adjusting sleeve with the communicating port on the cylinder body so as to ensure that the first reaction cavity is communicated with the second reaction cavity;

s7, starting a circulating pump, and injecting the feed liquid in the first reaction cavity and the second reaction cavity into the adjusting sleeve through the circulating pump through a mixing spray pipe pump;

s8, stopping the stirring mechanism and the circulating pump after 50 min;

and S9, after the material liquid in the reaction kettle is stable, closing the control valve on the material mixing spray pipe, opening the control valve on the material discharging pipe, then opening the circulating pump, and pumping the material liquid in the reaction kettle into a collecting container through the material discharging pipe by the circulating pump.
The method of claim 9, wherein: the fracturing cross-linking agent prepared by the method comprises zirconium hydroxide, fatty alcohol, organic peptide chelate and lauric acid polyoxyethylene ether.
The method of claim 10, wherein: the fracturing cross-linking agent consists of zirconium hydroxide, fatty alcohol, organic peptide chelate, lauric acid polyoxyethylene ether and water.