CN106281271A - Polynary complexed organo-metallic cross-linking agent and preparation method thereof - Google Patents

Polynary complexed organo-metallic cross-linking agent and preparation method thereof Download PDF

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Publication number
CN106281271A
CN106281271A CN201610589271.4A CN201610589271A CN106281271A CN 106281271 A CN106281271 A CN 106281271A CN 201610589271 A CN201610589271 A CN 201610589271A CN 106281271 A CN106281271 A CN 106281271A
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China
Prior art keywords
acid
add
cooh
aluminum chloride
preparation
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CN201610589271.4A
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Inventor
程杰成
周万富
王鑫
王力
郭红光
周泉
李庆松
王庆国
田亮
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Petrochina Co Ltd
Daqing Oilfield Co Ltd
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Petrochina Co Ltd
Daqing Oilfield Co Ltd
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Priority to CN201610589271.4A priority Critical patent/CN106281271A/en
Publication of CN106281271A publication Critical patent/CN106281271A/en
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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

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  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses one polynary complexed organo-metallic cross-linking agent relating to field of oilfield chemistry and preparation method thereof.Present invention mainly solves conventional metals cross-linking agent toxicity high, complex process, the problem that cost is high.The present invention it by malonic acid C3H4O4, citric acid C6H8O7, lactic acid C3H6O3, acetic acid CH3COOH, chromium trichloride CrCl3With aluminum chloride AlCl3And water composition, their percentage by weight is: malonic acid C3H4O4: 2 3%, citric acid C6H8O7: 1 2%, lactic acid C3H6O3: 4 5%, acetic acid CH3COOH:1 3%, chromium trichloride CrCl3: 7 8%, aluminum chloride AlCl3: 1 2%, water: 80 82%；It is simple that the present invention has preparation technology；Process safety is reliable, produces without dangerous, irritative gas in production process；Profile modification system good stability, the advantages such as endurance of cutting is good.

Description

Polynary complexed organo-metallic cross-linking agent and preparation method thereof
Technical field
The present invention relates to field of oilfield chemistry, particularly to polynary complexed organo-metallic cross-linking agent and preparation method thereof.
Background technology
Chrominum cross-linkage system is one of at present conventional crosslinked polymer system, its preparation process be broadly divided into oxidoreduction and Organic complex two kinds.Redox system is mainly reacted by bichromate and reducing agent and is prepared.Patent CN201310688950.3 In the oxidoreduction chromium cross linker mentioned and the preparation method of gel profile control agent thereof, it is to utilize bichromate to carry out oxidoreduction Reaction, during preparing chromium cross linker, needed raw material kind is many, and technological process is complicated, reacts and has irritative gas, and by In chromic hypertoxicity, easily cause environmental pollution, therefore also limit the application of this cross-linking agent preparation method.
Summary of the invention
It is an object of the invention to provide one to be environment-friendly and low-toxicity, react generated gelinite with crosslinked polymer and have higher Strength and stability, and preparation technology is simple, polynary complexed organo-metallic cross-linking agent that application cost is low and preparation method thereof.
The present invention by it by malonic acid C3H4O4, citric acid C6H8O7, lactic acid C3H6O3, acetic acid CH3COOH, chromium trichloride CrCl3With aluminum chloride AlCl3And water composition, their percentage by weight is: malonic acid C3H4O4: 2-3%, citric acid C6H8O7: 1-2%, lactic acid C3H6O3: 4-5%, acetic acid CH3COOH:1-3%, chromium trichloride CrCl3: 7-8%, aluminum chloride AlCl3: 1- 2%, water: 80-82%；
Its preparation method:
A, equipped with condensing tube, thermometer, Dropping funnel there-necked flask in add water: 80-90%, be subsequently adding malonic acid: 2- 3%, lactic acid: 4-5%, stirs, and then drips NaOH solution, adjusts pH to 4；It is warming up to 60 DEG C, while stirring, adds three Chlorizate chromium CrCl3: 7-8%, reaction 3 hours after having added；
B, add citric acid: 1-2%, be simultaneously added dropwise NaOH solution regulation pH value to 4, add aluminum chloride AlCl3: 1-2%, add Reaction 3 hours after complete；
C, product are cyan liquid, add acetic acid CH3COOH:1-3%；
D, if desired solidification make powder, and it is little that the liquid obtained in previous step being reacted joins standing 2 after stirring in 5 times amount ethanol Time, there is precipitation in bottle, obtain powder through sucking filtration evaporation liquid；Come again and obtain powder, 40 DEG C of oven for drying one day.
The action principle of the present invention: with the network of metal ion after being mixed according to different ratio by the acid of different complexation constants Close reaction, compare the cross linker system that single acid generates with complexing of metal ion, polynary crosslinking agent system metal ion More preferably, the stability of cross-linking agent is also more preferable simultaneously for slow release effect, owing to introducing a certain proportion of aluminium salt in metal ion, by adjusting The ratio of joint metal ion, it is possible to achieve gel rubber system all can plastic in the broader scope of pH value 6-9.
Polynary complexing metal cross-linking agent of the present invention has a characteristic that
1) needed raw material kind is less, and preparation technology is simple；
2) process safety is reliable, produces without dangerous, irritative gas in cross-linking agent production process；
3) profile modification system good stability, the gel that this cross-linking agent and polyacrylamide are cross-linked to form is placed in mill at a temperature of 45 DEG C In sand wide mouthed bottle, 180 days viscosity can arrive 20000mPa about s；
4) endurance of cutting is good, and the gel that this cross-linking agent and polyacrylamide are cross-linked to form adjusts device 6000 revs/min shearing through the most mixed After, little to plastic viscosity influence；
Detailed description of the invention: the invention will be further described below in conjunction with embodiment: it is by malonic acid C3H4O4, citric acid C6H8O7, lactic acid C3H6O3, acetic acid CH3COOH, chromium trichloride CrCl3With aluminum chloride AlCl3And water composition, their weight Percentage ratio is: malonic acid C3H4O4: 2-3%, citric acid C6H8O7: 1-2%, lactic acid C3H6O3: 4-5%, acetic acid CH3COOH:1-3%, three Chlorizate chromium CrCl3: 7-8%, aluminum chloride AlCl3: 1-2%, water: 80-82%；
Its preparation method:
A, equipped with condensing tube, thermometer, Dropping funnel there-necked flask in add water: 80-90%, be subsequently adding malonic acid: 2- 3%, lactic acid: 4-5%, stirs, and then drips NaOH solution, adjusts pH to 4；It is warming up to 60 DEG C, while stirring, adds three Chlorizate chromium CrCl3: 7-8%, reaction 3 hours after having added；
B, add citric acid: 1-2%, be simultaneously added dropwise NaOH solution regulation pH value to 4, add aluminum chloride AlCl3: 1-2%, add Reaction 3 hours after complete；
C, product are cyan liquid, add acetic acid CH3COOH:1-3%；
D, if desired solidification make powder, and it is little that the liquid obtained in previous step being reacted joins standing 2 after stirring in 5 times amount ethanol Time, there is precipitation in bottle, obtain powder through sucking filtration evaporation liquid；Come again and obtain powder, 40 DEG C of oven for drying one day.
Embodiment 1: the present embodiment is by malonic acid C3H4O4, citric acid C6H8O7, lactic acid C3H6O3, acetic acid CH3COOH, trichlorine Change chromium CrCl3With aluminum chloride AlCl3And water composition.Their percentage by weight is: malonic acid C3H4O4: 2%, citric acid C6H8O7: 1%, lactic acid C3H6O3: 4%, acetic acid CH3COOH:2%, chromium trichloride CrCl3: 8% and aluminum chloride AlCl3: 1%, water: 82%, obtain the polynary crosslinking agent aqueous solution of 18%.
The manufacture method of the present invention is:
A, equipped with condensing tube, thermometer, Dropping funnel there-necked flask in add water: 82%, be subsequently adding malonic acid: 2%, breast Acid: 4%, stirs, then dropping 2ml NaOH solution, adjusts pH to 4.It is warming up to 60 DEG C, while stirring, adds tri-chlorination Chromium CrCl3: 8%, reaction 3 hours after having added；
B, add citric acid: 1%, be simultaneously added dropwise 1ml NaOH solution regulation pH value to 4, add aluminum chloride AlCl3: 1%, add Reaction 3 hours after complete；
C, product are cyan liquid, add acetic acid CH3COOH:2%；Stir.
Embodiment 2: the present embodiment is by malonic acid C3H4O4, citric acid C6H8O7, lactic acid C3H6O3, acetic acid CH3COOH, trichlorine Change chromium CrCl3With aluminum chloride AlCl3And water composition.Their percentage by weight is: malonic acid C3H4O4: 2%, citric acid C6H8O7: 1%, lactic acid C3H6O3: 4%, acetic acid CH3COOH:3%, chromium trichloride CrCl3: 7% and aluminum chloride AlCl3: 2%, water: 81%, obtain the polynary crosslinking agent aqueous solution of 19%.
The manufacture method of the present invention is:
A, equipped with condensing tube, thermometer, Dropping funnel there-necked flask in add water: 81%, be subsequently adding malonic acid: 2%, breast Acid: 4%, stirs, then dropping 2ml NaOH solution, adjusts pH to 4.It is warming up to 60 DEG C, while stirring, adds tri-chlorination Chromium CrCl3: 7%, reaction 3 hours after having added；
B, add citric acid: 1%, be simultaneously added dropwise 1ml NaOH solution regulation pH value to 4, add aluminum chloride AlCl3: 2%, add Reaction 3 hours after complete；
C, product are cyan liquid, add acetic acid CH3COOH:3%；Stir.
Embodiment 3: the present embodiment is by malonic acid C3H4O4, citric acid C6H8O7, lactic acid C3H6O3, acetic acid CH3COOH, trichlorine Change chromium CrCl3With aluminum chloride AlCl3And water composition.Their percentage by weight is: malonic acid C3H4O4: 2%, citric acid C6H8O7: 1%, lactic acid C3H6O3: 5%, acetic acid CH3COOH:3%, chromium trichloride CrCl3: 8% and aluminum chloride AlCl3: 1%, water: 80%, obtain the polynary crosslinking agent aqueous solution of 20%.
The manufacture method of the present invention is:
A, equipped with condensing tube, thermometer, Dropping funnel there-necked flask in add water: 80%, be subsequently adding malonic acid: 2%, breast Acid: 5%, stirs, then dropping 3ml NaOH solution, adjusts pH to 4.It is warming up to 60 DEG C, while stirring, adds tri-chlorination Chromium CrCl3: 8%, reaction 3 hours after having added；
B, add citric acid: 1%, be simultaneously added dropwise 1ml NaOH solution regulation pH value to 4, add aluminum chloride AlCl3: 1%, add Reaction 3 hours after complete；
C, product are cyan liquid, add acetic acid CH3COOH:3%；Stir.

Claims (1)

  1. The most yuan of complexed organo-metallic cross-linking agent and preparation method thereof, it is characterised in that: a kind of polynary complexed organo-metallic cross-links Agent, it is by malonic acid C3H4O4, citric acid C6H8O7, lactic acid C3H6O3, acetic acid CH3COOH, chromium trichloride CrCl3And aluminum chloride AlCl3And water composition, their percentage by weight is: malonic acid C3H4O4: 2-3%, citric acid C6H8O7: 1-2%, lactic acid C3H6O3: 4-5%, acetic acid CH3COOH:1-3%, chromium trichloride CrCl3: 7-8%, aluminum chloride AlCl3: 1-2%, water: 80-82%；
    Its preparation method:
    A, equipped with condensing tube, thermometer, Dropping funnel there-necked flask in add water: 80-90%, be subsequently adding malonic acid: 2- 3%, lactic acid: 4-5%, stirs, and then drips NaOH solution, adjusts pH to 4；It is warming up to 60 DEG C, while stirring, adds three Chlorizate chromium CrCl3: 7-8%, reaction 3 hours after having added；
    B, add citric acid: 1-2%, be simultaneously added dropwise NaOH solution regulation pH value to 4, add aluminum chloride AlCl3: 1-2%, add Reaction 3 hours after complete；
    C, product are cyan liquid, add acetic acid CH3COOH:1-3%；
    D, if desired solidification make powder, and it is little that the liquid obtained in previous step being reacted joins standing 2 after stirring in 5 times amount ethanol Time, there is precipitation in bottle, obtain powder through sucking filtration evaporation liquid；Come again and obtain powder, 40 DEG C of oven for drying one day.
CN201610589271.4A 2016-07-26 2016-07-26 Polynary complexed organo-metallic cross-linking agent and preparation method thereof Pending CN106281271A (en)

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CN108517043A (en) * 2018-04-18 2018-09-11 中国石油天然气股份有限公司 A kind of polymer gel crosslinking agent that achievable gelation time is controllable
CN109735318A (en) * 2019-01-21 2019-05-10 克拉玛依中科恒信科技有限责任公司 A kind of pressure break enhanced type controllable cross-linking agent and preparation method thereof
CN110105938A (en) * 2019-05-14 2019-08-09 中国石油大学(华东) A kind of high intensity retarded crosslinking chromium gel and preparation method thereof

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108517043A (en) * 2018-04-18 2018-09-11 中国石油天然气股份有限公司 A kind of polymer gel crosslinking agent that achievable gelation time is controllable
CN108517043B (en) * 2018-04-18 2021-03-09 中国石油天然气股份有限公司 Polymer gel crosslinking agent capable of realizing controllable gelling time
CN109735318A (en) * 2019-01-21 2019-05-10 克拉玛依中科恒信科技有限责任公司 A kind of pressure break enhanced type controllable cross-linking agent and preparation method thereof
CN110105938A (en) * 2019-05-14 2019-08-09 中国石油大学(华东) A kind of high intensity retarded crosslinking chromium gel and preparation method thereof
CN110105938B (en) * 2019-05-14 2020-09-29 中国石油大学(华东) High-strength slow-crosslinking chromium jelly and preparation method thereof

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