CN111269676A - Strong acid resistant and fast-curing phosphate-based composite plugging agent - Google Patents

Strong acid resistant and fast-curing phosphate-based composite plugging agent Download PDF

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Publication number
CN111269676A
CN111269676A CN201811469701.4A CN201811469701A CN111269676A CN 111269676 A CN111269676 A CN 111269676A CN 201811469701 A CN201811469701 A CN 201811469701A CN 111269676 A CN111269676 A CN 111269676A
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China
Prior art keywords
agent
coupling agent
parts
silane coupling
plugging
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Pending
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CN201811469701.4A
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Chinese (zh)
Inventor
黄继庆
程永喜
方涛
索志勇
刘朝阳
王成刚
甄江涛
郭伟
刘旭
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Beijing Institute of Aerospace Testing Technology
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Beijing Institute of Aerospace Testing Technology
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Priority to CN201811469701.4A priority Critical patent/CN111269676A/en
Publication of CN111269676A publication Critical patent/CN111269676A/en
Pending legal-status Critical Current

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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
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J161/00—Adhesives based on condensation polymers of aldehydes or ketones; Adhesives based on derivatives of such polymers
    • C09J161/04—Condensation polymers of aldehydes or ketones with phenols only
    • C09J161/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08—Macromolecular additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/32—Phosphorus-containing compounds
    • C08K2003/329—Phosphorus containing acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Sealing Material Composition (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention relates to a strong acid resistant phosphate-based composite plugging agent capable of being rapidly cured. The plugging agent consists of A, B components, and the formula of each component is as follows according to parts by weight: part A: 70-80 parts of phenolic resin; 5-20 parts of a toughening agent; 30-40% of aluminum oxide; filler powder: 1-15; and part B: 10-50 parts of a curing agent; 5-25 parts of a coupling agent; 1-10 parts of an accelerator; 10-15 parts of phosphoric acid. Before plugging, the AB two parts are mixed at normal temperature and then coated on a metal plate, and the metal plate is forcibly pressed on a leakage point to be cured for 1-5 minutes, so that the plugging effect can be achieved. The composite plugging agent has excellent strong acid resistance, acid-resistant organic solvent resistance and high temperature resistance after being cured, has high adhesion to metal, and is suitable for quick adhesive plugging when equipment such as pipelines, tank bodies, flanges and the like of strong acid media and strong organic chemicals leak.

Description

Strong acid resistant and fast-curing phosphate-based composite plugging agent
Technical Field
The invention belongs to the technical field of leakage stoppage, and particularly relates to a preparation method of a fast-curing phenolic aldehyde modified phosphate-based composite leakage stoppage agent.
Background
The plugging agent is a binder which directly isolates a leakage medium from the outside, and has the advantages of excellent chemical stability, use temperature resistance, good binding power, dense texture, strong impermeability, high strength after curing, and capability of meeting the requirements of rapid curing in technical operation and the like. The running, the overflowing, the dripping and the leaking of some strong corrosive media such as concentrated nitric acid, concentrated sulfuric acid, concentrated hydrochloric acid and the like in the industry are difficult to solve. At present, a plurality of units at home and abroad compete with each other to research and develop a new plugging agent so as to solve the problem. The plugging agent for strong acid and strong corrosive media such as concentrated nitric acid, concentrated sulfuric acid, concentrated hydrochloric acid and the like is mainly divided into two categories, the first category is the plugging agent taking inorganic materials or inert materials as main bodies, such as water glass, quick cement, polytetrafluoroethylene and the like, the plugging agent has good material compatibility with strong acid but small adhesive force, and the plugging agent is generally used by adopting an injection type plugging process. However, the use of such lost circulation agents is very limited for leak locations that are not easily clamped. The second type is organic adhesive, such as resin type polyacrylate, phenolic resin, rubber type styrene butadiene rubber, butyl rubber, silicon rubber, etc. the plugging agent has great adhesion with the matrix, but has poor material compatibility with strong corrosive media such as strong acid, etc. Compared with other organic plugging agents, the phenolic resin plugging agent has the advantages of high cohesiveness, high chemical resistance, wide use temperature, low shrinkage rate and capability of being combined with other modifiers, but the compatibility with strong corrosive media such as concentrated nitric acid and concentrated sulfuric acid is still poor, and the acid-resistant phenolic resin plugging agent on the market at present can be broken and decomposed within 3 hours of soaking in strong acid, so that the development of the plugging agent which has high adhesive force with a metal matrix, high compatibility with strong acid media such as concentrated nitric acid, concentrated sulfuric acid and concentrated hydrochloric acid and can be quickly cured at room temperature is imperative.
Disclosure of Invention
The invention provides a strong acid-resistant phosphate-based composite plugging agent capable of being rapidly cured, which is divided into a part A and a part B which are separated from each other, and the specific formula is as follows in parts by mass:
part A:
phenolic resin, 70-80
Toughening agent, 5-20
30 to 40 parts of aluminum oxide
Acid-resistant filler powder: 1-15;
and part B:
curing agent, 10-50
Coupling agent, 5-25
Accelerant, 1-10
10 to 15 parts of phosphoric acid, H3PO4And (4) measuring the mass.
Wherein the curing agent is selected from 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane, diethylenetriamine, triethylenetetramine, tetraethylenepentamine or polythiol curing agent.
Wherein the accelerator is selected from benzyl dimethylamine, bicyclic amidine, thiourea, 2-methylimidazolium urea or 2-ethyl-4-methylimidazole, etc.
Wherein the toughening agent is selected from carboxyl-terminated liquid nitrile rubber, hydroxyl-terminated liquid nitrile rubber, liquid polysulfide rubber, liquid polybutadiene, chlorosulfonated polyethylene, copolymerized nylon, polyetherimide or polyether glycol carbonyl styrene-butadiene latex.
Wherein the coupling agent is selected from KH-550 silane coupling agent, KH-551 silane coupling agent, KH-560 silane coupling agent, KH-570 silane coupling agent, KH-580 silane coupling agent, KH-590 silane coupling agent, B-201 silane coupling agent, A-151 silane coupling agent, A-171 silane coupling agent, MTPS silane coupling agent or VTPS silane coupling agent.
Wherein the acid-resistant filler powder is selected from silicon micropowder, asbestos powder, mica, graphite powder, silicon dioxide, titanium dioxide, polytetrafluoroethylene ultrafine powder or portland cement.
Wherein the filler powder also comprises FeS24-12 parts of powder.
The application method of the strong acid resistant and fast-curing phosphate-based composite plugging agent is very simple, the AB components are mixed and then coated on the metal plate, and the metal plate is pressed on a leakage point forcibly and cured for a period of time, so that the plugging effect can be achieved.
The invention has the technical advantages that:
the plugging agent has excellent strong acid resistance, and the solidified sample of the plugging agent is soaked in concentrated sulfuric acid, concentrated nitric acid and concentrated hydrochloric acid respectively, and has no obvious change after being soaked for one week. The traditional acid-resistant plugging agent is broken and dissolved within 3 hours of being soaked in concentrated sulfuric acid, concentrated nitric acid and concentrated hydrochloric acid. Furthermore, the lost circulation additive of the present invention is particularly suitable for use in a dinitrogen tetroxide propellant for plugging leaks.
The plugging agent has quick curing capability, A, B part can be cured after being mixed for 2 minutes, and the traditional acid-resistant plugging agent can be cured after at least 10 minutes.
The plugging agent disclosed by the invention has stronger adhesive force after being completely cured, and the tensile shear strength of metal to metal reaches more than 5MPa after the plugging agent is cured for 1 hour at room temperature by adopting a test method of determining the tensile shear strength (rigid material to rigid material) of GB/T7124-2008 adhesive.
In the present invention, FeS is used in the part A2When powdered, the plugging effect is unexpectedly further enhanced, see in particular the examples section.
Drawings
None.
Detailed Description
Examples 1 to 3
Parts a and B in each example were prepared with the compositions shown in table 1 below, and leak plugging tests were performed under the test conditions and the test results shown in table 2 below.
Figure BSA0000175122020000031
TABLE 2
Figure BSA0000175122020000032
Example 4
This example has essentially the same composition as example 1, except that 5g of FeS has been added to part A2The leakage stoppage test still takes concentrated sulfuric acid as an example, and the unexpected discovery that the leakage stoppage time can be reduced to 1 minute, and the adhesive force after complete curing is measured by GB/T7124-2008 and can reach 18.7MPa, which shows that FeS2The specific reason is not detailed, and the S probably generated after the FeS2 meets acid is guessed2 2-The ions may be cross-linked with each other under plugging conditions to form long-chain polysulfide ions S2x 2-Intertwine with the inorganic polyphosphate polymer chains, and serve to promote crosslinking.

Claims (8)

1. The strong acid resistant phosphate-based composite plugging agent capable of being cured quickly is characterized by being divided into a part A and a part B which are separated from each other, and the specific formula comprises the following components in parts by mass:
part A:
phenolic resin, 70-80
Toughening agent, 5-20
30 to 40 parts of aluminum oxide
Acid-resistant filler powder: 1-15;
and part B:
curing agent, 10-50
Coupling agent, 5-25
Accelerant, 1-10
10-15 parts of phosphoric acid.
2. The composite lost circulation additive of claim 1, wherein the toughening agent is selected from carboxyl-terminated liquid nitrile rubber, hydroxyl-terminated liquid nitrile rubber, liquid polysulfide rubber, liquid polybutadiene, chlorosulfonated polyethylene, copolymerized nylon, polyetherimide or polyether glycol carbonyl styrene butadiene latex.
3. The composite plugging agent of claim 1, wherein the acid-resistant filler powder is selected from silica micropowder, asbestos powder, mica, graphite powder, silica, titanium dioxide, polytetrafluoroethylene micropowder or portland cement.
4. The composite lost circulation additive of claim 1, wherein the curing agent is selected from 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane, diethylenetriamine, triethylenetetramine, tetraethylenepentamine or polythiol curing agents.
5. The composite plugging agent according to claim 1, wherein the coupling agent is selected from a KH-550 silane coupling agent, a KH-551 silane coupling agent, a KH-560 silane coupling agent, a KH-570 silane coupling agent, a KH-580 silane coupling agent, a KH-590 silane coupling agent, a B-201 silane coupling agent, an a-151 silane coupling agent, an a-171 silane coupling agent, an MTPS silane coupling agent, or a VTPS silane coupling agent.
6. The composite plugging agent of claim 1, wherein the accelerator is selected from the group consisting of benzyldimethylamine, bicyclic amidine, thiourea, 2-methylimidazolium urea, 2-ethyl-4-methylimidazole, and the like.
7. The composite plugging agent of claim 1, wherein the part a further comprises FeS24-12 parts of powder.
8. Use of the composite plugging agent according to claim 1 for plugging leaking sulfuric acid, nitric acid, hydrochloric acid, phosphoric acid or dinitrogen tetroxide.
CN201811469701.4A 2018-12-04 2018-12-04 Strong acid resistant and fast-curing phosphate-based composite plugging agent Pending CN111269676A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116769400A (en) * 2023-05-19 2023-09-19 广州力盾环保工程有限公司 Plugging material for dry suction tower flue gas pipeline and plugging method thereof

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Publication number Priority date Publication date Assignee Title
JPS6279282A (en) * 1985-10-02 1987-04-11 Sunstar Giken Kk Resin composition
CN1097207A (en) * 1994-03-09 1995-01-11 河南省华豫科技实业总公司 Agent for stopping-leaks and scaling of water tank
CN101440268A (en) * 2008-12-30 2009-05-27 黑龙江省科学院石油化学研究院 Low temperature curing high temperature resistant inorganic / organic hybridization epoxy adhesive and preparation thereof
CN101875830A (en) * 2009-11-23 2010-11-03 黑龙江省科学院石油化学研究院 Phenolic resin/phosphate hybrid adhesive and preparation method thereof
CN103113841A (en) * 2012-12-07 2013-05-22 北京航天试验技术研究所 Preparation method of strong-acid-resistant epoxy resin quick plugging agent

Patent Citations (5)

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Publication number Priority date Publication date Assignee Title
JPS6279282A (en) * 1985-10-02 1987-04-11 Sunstar Giken Kk Resin composition
CN1097207A (en) * 1994-03-09 1995-01-11 河南省华豫科技实业总公司 Agent for stopping-leaks and scaling of water tank
CN101440268A (en) * 2008-12-30 2009-05-27 黑龙江省科学院石油化学研究院 Low temperature curing high temperature resistant inorganic / organic hybridization epoxy adhesive and preparation thereof
CN101875830A (en) * 2009-11-23 2010-11-03 黑龙江省科学院石油化学研究院 Phenolic resin/phosphate hybrid adhesive and preparation method thereof
CN103113841A (en) * 2012-12-07 2013-05-22 北京航天试验技术研究所 Preparation method of strong-acid-resistant epoxy resin quick plugging agent

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上海市土木工程学会 等: "《图说隧道与地铁工程防水技术》", 31 May 2018, 同济大学出版社 *
张玉龙: "《粘接技术手册》", 31 August 2001, 中国轻工业出版社 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116769400A (en) * 2023-05-19 2023-09-19 广州力盾环保工程有限公司 Plugging material for dry suction tower flue gas pipeline and plugging method thereof
CN116769400B (en) * 2023-05-19 2024-04-19 广州力盾环保工程有限公司 Plugging material for dry suction tower flue gas pipeline and plugging method thereof

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