CN106565128B - A kind of polyester ethers defoaming agent and its preparation method and application - Google Patents
A kind of polyester ethers defoaming agent and its preparation method and application Download PDFInfo
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- CN106565128B CN106565128B CN201610918592.4A CN201610918592A CN106565128B CN 106565128 B CN106565128 B CN 106565128B CN 201610918592 A CN201610918592 A CN 201610918592A CN 106565128 B CN106565128 B CN 106565128B
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- defoaming agent
- cement slurry
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- catalyst
- polyester ethers
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Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/28—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/32—Polyethers, e.g. alkylphenol polyglycolether
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/329—Polymers modified by chemical after-treatment with organic compounds
- C08G65/331—Polymers modified by chemical after-treatment with organic compounds containing oxygen
- C08G65/332—Polymers modified by chemical after-treatment with organic compounds containing oxygen containing carboxyl groups, or halides, or esters thereof
- C08G65/3322—Polymers modified by chemical after-treatment with organic compounds containing oxygen containing carboxyl groups, or halides, or esters thereof acyclic
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/50—Defoamers, air detrainers
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Polyethers (AREA)
Abstract
The invention belongs to technical field of oilfield chemistry, more particularly to a kind of polyester ethers defoaming agent and its preparation method and application, polyester ethers defoaming agent of the invention is the modified of polyethers defoaming agent, both polyethers defoaming agent high temperature resistant had been saved after the esterification of polyether antifoam agent, had been easily dispersed, the advantages that surface tension is low, stability is good, again because the hydrogen bond of hydrone and polyoxyethylene interchain after esterification is weakened, so that its lipophilicity increases, hydrophily further decreases, advantageously reduce surface tension, get higher its activity, defoaming capacity enhancing.
Description
Technical field
The invention belongs to technical field of oilfield chemistry, and in particular to a kind of polyester ethers defoaming agent and preparation method thereof and answer
With.
Background technique
Oil-well cement defoaming agent is many kinds of at present, and performance is totally different, is divided into mineral oils, organosilicon by the composition of defoaming agent
Type, polyether-type, silicon are ether mixed.
Mineral oil defoaming agent is substituted due to bad dispersibility in water；Organic silicon defoaming agent generally comprises poly- diformazan
The disadvantages of products such as radical siloxane have the characteristics that antifoaming speed is fast, foam inhibition is preferable, but price is high, not soluble in water causes universal
Using limited；And polyether-type defoaming agent is with nontoxic, defoaming effect is excellent, thermal stability is good, scattered in nonirritant and water
The features such as, industry, food, in terms of be widely used.
Although polyether-type defoaming agent is widely used, because of the relationship of selectivity, some fields cannot still be used so far.
Summary of the invention
The purpose of the present invention is develop the polyethet surfactant of different structure ester is made by being esterified polyethers
Ether type defoaming agent, to widen its application range.
For this purpose, the present invention provides a kind of polyester ethers defoaming agent, the defoaming agent by following mass fraction component
Under the action of catalyst obtained by esterification:
8~18 parts of polyethers；
5~15 parts of organic acid.
The polyethers is polyoxypropylene ethylene oxide glycerin ether；The organic acid is lauric acid；The catalyst
It is the concentrated sulfuric acid.
The defoaming agent the preparation method is as follows:
Take 5~15 parts of 8~18 parts of polyethers, organic acid addition catalyst by mass fraction, at a temperature of 60~100 DEG C into
Row esterification, reaction time 2h~8h, esterification are cooled down after the completion, and adjust pH value 5~8, then with saturation
It is required defoaming agent that sodium chloride solution, which removes impurity,.
The catalyst is the concentrated sulfuric acid, and the concentration of catalyst is the 0.2-1.0% for accounting for the amount of reactant total material.
The defoaming agent the preparation method is as follows:
9 parts of polyoxypropylene ethylene oxide glycerin ether, 13 parts of lauric acid are taken by mass fraction, adds total moles quality
0.6% concentrated sulfuric acid is heated to catalyst at 90 DEG C and is dissolved completely in polyoxypropylene ethylene oxide glycerin ether, reaction time 7h,
Acid value measuring is carried out per sampling every other hour during the reaction, to determine system esterification yield, when rate to be esterified is constant, is cooled to
60 DEG C, KOH aqueous solution is added and is neutralized, adjusts pH value 7, being extracted with saturated sodium chloride solution remove impurity later is institute
The defoaming agent needed.
The polyester ethers defoaming agent is defoamed for cement slurry.
The polyester ethers defoaming agent is used for the concrete mode of cement slurry defoaming are as follows: by polyester ethers defoaming agent to account for water
0.05% deal and cement slurry of quality of mud fluid are mixed to form new cement slurry.
Beneficial effects of the present invention: this polyester ethers defoaming agent provided by the invention and its preparation method and application is
The modified of polyethers defoaming agent had both saved polyethers defoaming agent high temperature resistant, had been easily dispersed, surface after the esterification of polyether antifoam agent
The advantages that tension is low, stability is good, and because the hydrogen bond of hydrone and polyoxyethylene interchain after esterification is weakened, so that it is lipophilic
Increase, hydrophily further decreases, advantageously reduces surface tension, get higher its activity, defoaming capacity enhancing.
Specific embodiment
Embodiment 1:
This city embodiment provides a kind of polyester ethers defoaming agent, and the defoaming agent is being urged by the component of following mass fraction
Agent acts on obtained by lower esterification:
8~18 parts of polyethers；
5~15 parts of organic acid.
Wherein, polyethers is polyoxypropylene ethylene oxide glycerin ether；The organic acid is lauric acid；The catalyst is
The concentrated sulfuric acid.
Polyester ethers defoaming agent in the present embodiment is obtained after esterification, and polyethers defoaming had both been saved after esterification
Agent high temperature resistant is easily dispersed, the advantages that surface tension is low, stability is good, and because of hydrone after esterification and polyoxyethylene interchain
Hydrogen bond is weakened, so that its lipophilicity increases, hydrophily further decreases, advantageously reduces surface tension, get higher its activity,
Defoaming capacity enhancing.
Embodiment 2:
Defoaming agent in above-described embodiment the preparation method is as follows:
Take 5~15 parts of 8~18 parts of polyethers, organic acid addition catalyst by mass fraction, at a temperature of 60~100 DEG C into
Row esterification, reaction time 2h~8h, esterification are cooled down after the completion, and adjust pH value 5~8, then with saturation
It is required defoaming agent that sodium chloride solution, which removes impurity,.
Wherein, catalyst is the concentrated sulfuric acid, and the concentration of catalyst is the 0.2-1.0% for accounting for the amount of reactant total material.
More specifically, defoaming agent the preparation method is as follows:
9 parts of polyoxypropylene ethylene oxide glycerin ether, 13 parts of lauric acid are taken by mass fraction, adds total moles quality
0.6% concentrated sulfuric acid is heated to catalyst at 90 DEG C and is dissolved completely in polyoxypropylene ethylene oxide glycerin ether, reaction time 7h,
Acid value measuring is carried out per sampling every other hour during the reaction, to determine system esterification yield, when rate to be esterified is constant, is cooled to
60 DEG C, KOH aqueous solution is added and is neutralized, adjusts pH value 7, being extracted with saturated sodium chloride solution remove impurity later is institute
The defoaming agent needed.
Embodiment 3:
The polyester ethers defoaming agent referred in above-described embodiment 1 and embodiment 2 can be used for cement slurry defoaming.
Polyester ethers defoaming agent is used for the concrete mode of cement slurry defoaming are as follows: by polyester ethers defoaming agent to account for cement slurry matter
0.05% deal and cement slurry of amount are mixed to form new cement slurry.
The modified polyester ethers defoaming agent of development is defoamed for cement slurry, is added defoaming agent (account for cement amount 0.05%)
The density recovery rate of cement slurry is 90% or more afterwards, and temperature resistance is up to 120 DEG C, on the compression strength of cement slurry without influence, no secondary work
With.It is good with cement additive compatibility, the performance requirement of cement slurry under different temperatures can be met, can be eliminated in cement slurry
Foam, and the performance of other additives is not influenced, there is good application prospect.
It is illustrated below in conjunction with this silicon ethers foam inhibitor of the specific real time data to the present embodiment.
Embodiment 4:
9 parts of polyoxypropylene ethylene oxide glycerin ether, 13 parts of lauric acid are taken by mass fraction, adds total moles quality
0.6% concentrated sulfuric acid is heated to catalyst at 90 DEG C and is dissolved completely in polyoxypropylene ethylene oxide glycerin ether, reaction time 7h,
Acid value measuring is carried out per sampling every other hour during the reaction, to determine system esterification yield, when rate to be esterified is constant, is cooled to
60 DEG C, KOH aqueous solution is added and is neutralized, adjusts pH value 7, being extracted with saturated sodium chloride solution remove impurity later is institute
The defoaming agent needed, obtained polyester ethers defoaming agent is added in cement slurry, and specific dosage is the 0.05% of cement slurry quality.
Obtained new cement slurry and original cement slurry are divided into point that multiple groups carry out compression strength, temperature, density
Analysis experiment, obtains the data in following table 1:
1: the first component cement of table starches compression strength, temperature, density experiment data
Embodiment 5:
18 parts of polyoxypropylene ethylene oxide glycerin ether, 5 parts of lauric acid are taken by mass fraction, adds the 1% of total moles quality
The concentrated sulfuric acid, be heated to catalyst at 100 DEG C and be dissolved completely in polyoxypropylene ethylene oxide glycerin ether, reaction time 8h,
Acid value measuring is carried out per sampling every other hour in reaction process, to determine system esterification yield, when rate to be esterified is constant, is cooled to 60
DEG C, KOH aqueous solution is added and is neutralized, adjusts pH value 8, is extracted later with saturated sodium chloride solution needed for removing impurity as
Defoaming agent, obtained polyester ethers defoaming agent is added in cement slurry, specific dosage be cement slurry quality 0.05%.
Obtained new cement slurry and original cement slurry are divided into point that multiple groups carry out compression strength, temperature, density
Analysis experiment, obtains the data in following table 2:
2: the second component cement of table starches compression strength, temperature, density experiment data
Embodiment 6:
8 parts of polyoxypropylene ethylene oxide glycerin ether, 15 parts of lauric acid are taken by mass fraction, adds total moles quality
0.2% concentrated sulfuric acid is heated to catalyst at 90 DEG C and is dissolved completely in polyoxypropylene ethylene oxide glycerin ether, reaction time 3h,
Acid value measuring is carried out per sampling every other hour during the reaction, to determine system esterification yield, when rate to be esterified is constant, is cooled to
60 DEG C, KOH aqueous solution is added and is neutralized, adjusts pH value 6, being extracted with saturated sodium chloride solution remove impurity later is institute
The defoaming agent needed, obtained polyester ethers defoaming agent is added in cement slurry, and specific dosage is the 0.05% of cement slurry quality.
Obtained new cement slurry and original cement slurry are divided into point that multiple groups carry out compression strength, temperature, density
Analysis experiment, obtains the data in following table 3:
Table 3: third component cement slurry compression strength, temperature, density experiment data
By data in the above table 1, table 2 and table 3 it is found that the cement slurry of polyester ethers defoaming agent is added compared to common water
Mud, in the case where ordinary cement slurry temperature resistance only has 100 DEG C, be added the present embodiment polyester ethers defoaming agent may make it is new
Cement slurry temperature resistance is up to 120 DEG C；And the density recovery rate of cement slurry reaches 90% or more, from the resistance to compression of the above ordinary cement slurry
Intensity is compared with the cement slurry of the addition polyester ethers defoaming agent of the present embodiment, and compression strength is without side-effects without influence.
In conclusion this addition polyester ethers defoaming agent of the invention and cement additive compatibility are good, can meet
The performance requirement of cement slurry under different temperatures can eliminate the foam in cement slurry and influence the performance of other additives, have
Good application prospect.
The foregoing examples are only illustrative of the present invention, does not constitute the limitation to protection scope of the present invention, all
It is within being all belonged to the scope of protection of the present invention with the same or similar design of the present invention.
Claims (2)
1. a kind of application of polyester ethers defoaming agent in cement slurry defoaming, it is characterised in that: the defoaming agent is by following matter
The component of amount number is under the action of catalyst obtained by esterification:
8~18 parts of polyethers；
5~15 parts of organic acid；
The polyethers is polyoxypropylene ethylene oxide glycerin ether；The organic acid is lauric acid；The catalyst is dense
Sulfuric acid；
The defoaming agent the preparation method is as follows:
5~15 parts of 8~18 parts of polyethers, organic acid addition catalyst are taken by mass fraction, carries out ester at a temperature of 60~100 DEG C
Change reaction, reaction time 2h~8h, esterification is cooled down after the completion, and adjusts pH value 5~8, then with saturation chlorination
It is required defoaming agent that sodium solution extraction, which removes impurity,；
The concentration of the catalyst is the 0.2-1.0% for accounting for the amount of reactant total material；
The polyester ethers defoaming agent is used for the concrete mode of cement slurry defoaming are as follows: by polyester ethers defoaming agent to account for cement slurry
0.05% deal and cement slurry of quality are mixed to form new cement slurry.
2. application as described in claim 1, it is characterised in that: the defoaming agent the preparation method is as follows:
9 parts of polyoxypropylene ethylene oxide glycerin ether, 13 parts of lauric acid are taken by mass fraction, adds the 0.6% of the amount of total material
The concentrated sulfuric acid is heated to catalyst at 90 DEG C and is dissolved completely in polyoxypropylene ethylene oxide glycerin ether, and reaction time 7h is reacting
Acid value measuring is carried out per sampling every other hour in the process, to determine system esterification yield, when rate to be esterified is constant, is cooled to 60 DEG C,
KOH aqueous solution is added to be neutralized, adjusts pH value 7, it is required for being extracted with saturated sodium chloride solution remove impurity later
Defoaming agent.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610918592.4A CN106565128B (en) | 2016-10-21 | 2016-10-21 | A kind of polyester ethers defoaming agent and its preparation method and application |
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| CN201610918592.4A CN106565128B (en) | 2016-10-21 | 2016-10-21 | A kind of polyester ethers defoaming agent and its preparation method and application |
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| CN106565128A CN106565128A (en) | 2017-04-19 |
| CN106565128B true CN106565128B (en) | 2019-04-16 |
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| CN102286146A (en) * | 2011-05-04 | 2011-12-21 | 湖北富邦科技股份有限公司 | Preparation method of defoaming agent for producing phosphoric acid by wet process |
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Effective date of registration: 20201029 Address after: 100007 Dongcheng District, Dongzhimen, China, North Street, No. 9 Oil Mansion, No. Patentee after: CHINA NATIONAL PETROLEUM Corp. Patentee after: CNPC Chuanqing Drilling Engineering Co.,Ltd. Address before: Company No. 151 Changqing building cementing Weiyang road 710021 Shaanxi city of Xi'an Province Patentee before: Changqing cementing company of CNPC Chuanqing Drilling Engineering Co.,Ltd. Patentee before: SHAANXI GUDE PETROLEUM ENGINEERING Co.,Ltd. |