CN101367928A - Alkene based amine polyether and method of preparing the same - Google Patents
Alkene based amine polyether and method of preparing the same Download PDFInfo
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Abstract
The invention discloses alkenylamines polyether, expressed by right constitutional formula, wherein, R1 is alkenyl with 3-6 carbon atoms; m, n, p and q are integers greater than 0, and m and n are not equal to 0 at the same time, and p and q are not equal to 0. The alkenylamines polyether has a double-branch structure, and can be used as poly carboxylic acid water reducing agent which has excellent slumping retention performance to concrete in synthesis of raw materials.
Description
Technical field
The present invention relates to a kind of polyethers, be specifically related to a kind of alkenyl amine polyethers and preparation method thereof.
Background technology
At present, fast development along with concrete industry, utilize cement water reducing agent to prepare the attention that high performance concrete more and more obtains people, wherein, polycarboxylate dehydragent is the focus of studying both at home and abroad in recent years, it has the advantage of a lot of uniquenesses, such as have good slump retentivity at low water-cement ratio, different cement is had good relatively adaptability etc.
In the prior art, the raw material that is used for synthesizing polycarboxylate superplasticizer mainly contains polyoxyethylene glycol, methoxy poly (ethylene glycol) ether, allyl polyglycol ether, methoxy poly (ethylene glycol) ether (methyl) acrylate etc.In order to improve the performance of polycarboxylate dehydragent, for example water-reducing property and slump retentivity are necessary to develop new raw material, in order to the preparation polycarboxylate dehydragent.
Summary of the invention
The purpose of this invention is to provide a kind of alkenyl amine polyethers and preparation method thereof, it can be used as raw material and is used for synthesizing polycarboxylate superplasticizer.
To achieve the above object of the invention, the technical solution used in the present invention is: a kind of alkenyl amine polyethers, adopt following structural to express:
Wherein, R
1Thiazolinyl for carbonatoms 3～6; M, n, p and q are the integer more than or equal to 0, and m and n be not 0 simultaneously, and p and q are not 0 simultaneously.
Above, C
2H
4O is an oxyethylene group, C
3H
6O is an oxypropylene group; M, n, p, q represent the average addition mole number of each oxyalkylene group.For a side chain of above-mentioned chemical formula, m and n are not 0 simultaneously, and be meant that this side chain comprises following 3 kinds of situations: (1) m is 0 o'clock, is the polyoxypropylene base; (2) n is 0 o'clock, is polyoxyethylene groups; (3) m, n all are not 0 o'clock, are the mixing copolymerization chain of oxypropylene group and oxyethylene group; Another side chain of chemical formula also is like this; For whole chemical formula, these two side chains can be identical or different.
Alkenyl amine polyethers of the present invention can adopt following method preparation:
(1) under negative pressure, in reactor, add alkenyl amine, start outer circulation, behind the air in the inflated with nitrogen replacement reaction kettle, below the temperature adjustment to 20 ℃, vacuumize then, again material in reactor is heated to 130～140 ℃ after, add epoxy alkane and also carry out circulating reaction, temperature of reaction is 130～170 ℃, reaction pressure is less than 0.4MPa, adds the back 130～170 ℃ of following insulation reaction at least 20 minutes, and cooling is cooled to 80～90 ℃ again; Wherein, the mol ratio of alkenyl amine and epoxy alkane is 1:2～1:4;
(2) aforesaid reaction vessel is vacuumized after, suck catalyzer, the air in the inflated with nitrogen replacement reaction kettle again, vacuumize, be heated to 130～140 ℃, add epoxy alkane then and carry out circulating reaction, temperature of reaction is 130～170 ℃, reaction pressure is less than 0.4MPa, add the back till 130～170 ℃ of following insulation reaction at least 20 minutes no longer descend to reacting kettle inner pressure, cooling is cooled to 50～60 ℃ again, stops outer circulation, discharging promptly obtains described alkenyl amine polyethers; Wherein, the mol ratio of alkenyl amine and epoxy alkane is 1:9～1:66;
Wherein, catalyzer is sodium hydroxide solution or methanol solution of sodium methylate described in the step (2).
Optimized technical scheme, the alkenyl amine in the described step (1) and the mol ratio of epoxy alkane are 1:2.Be about to 1 mole alkenyl amine and 2 moles epoxy alkane reaction, make primary amine all change into tertiary amine---two (β-hydroxyalkyl) alkenyl amine, thus the difference of total amine value that has guaranteed time to go on foot the alkenyl amine polyethers of preparing and tertiary amine value is as far as possible little.
Before adding the epoxy alkane reactant, add a small amount of epoxy alkane earlier and carry out pre-reaction in described step (1) and the step (2).Carry out pre-reaction earlier, can further guarantee the steady and safety of reacting.
In the technique scheme, in described step (1), the temperature of reaction of addition of ethylene oxide is 160～170 ℃ separately, and the temperature of reaction of addition propylene oxide is 130～140 ℃ separately, and the temperature of reaction of both mixtures of addition is 130～150 ℃.
Alkenyl amine polyethers of the present invention is used for synthesizing polycarboxylate superplasticizer mainly as raw material.
Because the employing of technique scheme, compared with prior art, the present invention has following advantage:
1. the alkenyl amine polyethers of the present invention's acquisition has two branched structures, can be used as the synthetic polycarboxylate water-reducer that concrete is had excellent slump retentivity of raw material.
2. in the preparation method's of the present invention step (1), adopt the method for lower the temperature, vacuumizing again, close earlier ability heat temperature raising after the vacuum, creative.
3. the alkenyl amine polyethers color and luster that utilizes preparation method of the present invention to obtain is good, and total amine value and tertiary amine value difference are little, and two side chain length are even.
4. preparation method of the present invention is simple, and technology is controlled, and reacting balance safety only needed for two steps can obtain target compound.
Embodiment
Below in conjunction with embodiment the present invention is further described, but should limit protection scope of the present invention with this:
Embodiment one:
The allyl amine Soxylat A 25-7, its preparation method is as follows:
The first step under negative pressure, drop into 5.7 kilograms allyl amine in the outer circulation of clean exsiccant 200L atomizing still, starts canned-motor pump, and the air in the inflated with nitrogen displacement still below the temperature adjustment to 20 ℃, vacuumizes; Guarantee the pumpdown time more than 30 minutes, the stop pumping vacuum; Slowly material is heated to 130～140 ℃, stops heating, add a small amount of oxyethane from the reactor top-spray, treat that still pushes back backwardness, spraying adds oxyethane again, along with the adding of oxyethane, temperature in the material reaction, still progressively raises naturally, and the still internal pressure increases; Material is extracted out at the bottom of still by canned-motor pump in the still, after canned-motor pump pressurization, interchanger temperature adjustment, enters (with reacting ethylene oxide) the still after the atomizing of still top, is deposited at the bottom of the still again; Like this circulating reaction, 160～170 ℃ of control reaction temperature, pressure is less than 0.35Mpa, and the add-on of oxyethane is 8.8 kilograms altogether, after adding, till 160～170 ℃ of insulation reaction no longer descended to the still internal pressure more than 20 minutes; Be cooled to 80～90 ℃;
Second step, the reactor of the first step is vacuumized, under the condition of negative pressure, suck 0.2 kilogram of 50% sodium hydroxide solution as catalyzer, inflated with nitrogen is replaced the air in the still again, the limit vacuumizes, heat up in the limit, and temperature reaches 130～140 ℃, stops heating, guarantee the pumpdown time more than 30 minutes, the stop pumping vacuum; Add a small amount of oxyethane from the reactor top-spray, treat that still pushes back backwardness, spraying adds oxyethane again, and along with the adding of oxyethane, the temperature in the material reaction, still progressively raises naturally, and the still internal pressure increases.Material is extracted out at the bottom of still by canned-motor pump in the still, after canned-motor pump pressurization, interchanger temperature adjustment, enters (with reacting ethylene oxide) the still after the atomizing of still top, is deposited at the bottom of the still again; Like this circulating reaction, 160～170 ℃ of control reaction temperature, pressure is less than 0.35Mpa, and the add-on of oxyethane is 85.5 kilograms altogether, after adding, till 160～170 ℃ of insulation reaction no longer descended to the still internal pressure more than 20 minutes; Be cooled to 50～60 ℃, stop canned-motor pump, discharging.Can obtain described allyl amine Soxylat A 25-7.
Embodiment two:
The allyl amine Soxylat A 25-7, its preparation method is as follows:
The first step under negative pressure, drop into 5.7 kilograms allyl amine in the outer circulation of clean exsiccant 200L atomizing still, starts canned-motor pump, and the air in the inflated with nitrogen displacement still below the temperature adjustment to 20 ℃, vacuumizes; Guarantee the pumpdown time more than 30 minutes, the stop pumping vacuum; Slowly material is heated to 130～140 ℃, stops heating, add a small amount of oxyethane from the still top-spray, treat that still pushes back backwardness, spraying adds oxyethane again, along with the adding of oxyethane, material reaction, temperature in the still progressively raises naturally, the still internal pressure increases, and material is extracted out at the bottom of still by canned-motor pump in the still, after canned-motor pump pressurization, interchanger temperature adjustment, after the atomizing of still top, enter (with reacting ethylene oxide) the still, be deposited at the bottom of the still again; Like this circulating reaction, 160～170 ℃ of control reaction temperature, pressure is less than 0.35Mpa, and the add-on of oxyethane is 8.8 kilograms altogether, after adding, till 160～170 ℃ of insulation reaction no longer descended to the still internal pressure more than 20 minutes; Be cooled to 80～90 ℃;
Second step, the reactor of the first step is vacuumized, under the condition of negative pressure, suck 0.3 kilogram of 50% sodium hydroxide solution as catalyzer, inflated with nitrogen is replaced the air in the still again, the limit vacuumizes, heat up in the limit, and temperature reaches 130～140 ℃, stops heating, guarantee the pumpdown time more than 30 minutes, the stop pumping vacuum; Add a small amount of oxyethane from the still top-spray, treat that still pushes back backwardness, spraying adds oxyethane again, along with the adding of oxyethane, material reaction, temperature in the still progressively raises naturally, the still internal pressure increases, and material is extracted out at the bottom of still by canned-motor pump in the still, after canned-motor pump pressurization, interchanger temperature adjustment, after the atomizing of still top, enter (with reacting ethylene oxide) the still, be deposited at the bottom of the still again; Like this circulating reaction, 160～170 ℃ of control reaction temperature, pressure is less than 0.35Mpa, and the add-on of oxyethane is 135.5 kilograms altogether, after adding, till 160～170 ℃ of insulation reaction no longer descended to the still internal pressure more than 20 minutes; Be cooled to 50～60 ℃, stop canned-motor pump, discharging.Can obtain described allyl amine Soxylat A 25-7.
Embodiment three:
The allyl amine Soxylat A 25-7, its preparation method is as follows:
The first step under negative pressure, drop into 8.55 kilograms allyl amine in the outer circulation of clean exsiccant 200L atomizing still, starts canned-motor pump, and the air in the inflated with nitrogen displacement still below the temperature adjustment to 20 ℃, vacuumizes; Guarantee the pumpdown time more than 30 minutes, the stop pumping vacuum; Slowly material is heated to 130～140 ℃, stops heating, add a small amount of oxyethane from the still top-spray, treat that still pushes back backwardness, spraying adds oxyethane again, along with the adding of oxyethane, material reaction, temperature in the still progressively raises naturally, the still internal pressure increases, and material is extracted out at the bottom of still by canned-motor pump in the still, after canned-motor pump pressurization, interchanger temperature adjustment, after the atomizing of still top, enter (with reacting ethylene oxide) the still, be deposited at the bottom of the still again; Like this circulating reaction, 160～170 ℃ of control reaction temperature, pressure is less than 0.35Mpa, and the add-on of oxyethane is 13.2 kilograms altogether, after adding, till 160～170 ℃ of insulation reaction no longer descended to the still internal pressure more than 20 minutes; Be cooled to 80～90 ℃;
Second step, the reactor of the first step is vacuumized, under the condition of negative pressure, suck 0.2 kilogram of 50% sodium hydroxide solution as catalyzer, inflated with nitrogen is replaced the air in the still again, the limit vacuumizes, heat up in the limit, and temperature reaches 130～140 ℃, stops heating, guarantee the pumpdown time more than 30 minutes, the stop pumping vacuum; Add a small amount of oxyethane from the still top-spray, treat that still pushes back backwardness, spraying adds oxyethane again, along with the adding of oxyethane, material reaction, temperature in the still progressively raises naturally, the still internal pressure increases, and material is extracted out at the bottom of still by canned-motor pump in the still, after canned-motor pump pressurization, interchanger temperature adjustment, after the atomizing of still top, enter (with reacting ethylene oxide) the still, be deposited at the bottom of the still again; Like this circulating reaction, 160～170 ℃ of control reaction temperature, pressure is less than 0.35Mpa, and the add-on of oxyethane is 98.25 kilograms altogether, after adding, till 160～170 ℃ of insulation reaction no longer descended to the still internal pressure more than 20 minutes; Be cooled to 50～60 ℃, stop canned-motor pump, discharging.Can obtain described allyl amine Soxylat A 25-7.
With the allyl amine Soxylat A 25-7 that the foregoing description one to three obtains, respectively its color and luster, total amine value and tertiary amine value are measured result such as following table:
The determination data of table 1 allyl amine Soxylat A 25-7
As can be seen from the above table, the product color that the present invention obtains is good, and total amine value and tertiary amine value difference are little.
Embodiment four:
The allyl amine polyethenoxy ether, its preparation method is as follows:
The first step under negative pressure, drop into 5.7 kilograms allyl amine in the outer circulation of clean exsiccant 200L atomizing still, starts canned-motor pump, and the air in the inflated with nitrogen displacement still below the temperature adjustment to 20 ℃, vacuumizes; Guarantee the pumpdown time more than 30 minutes, the stop pumping vacuum; Slowly material is heated to 130～140 ℃, stops heating, add minor amount of propylene oxide from the still top-spray, treat that still pushes back backwardness, spraying adds propylene oxide again, along with the adding of propylene oxide, material reaction, temperature in the still progressively raises naturally, the still internal pressure increases, and material is extracted out at the bottom of still by canned-motor pump in the still, after canned-motor pump pressurization, interchanger temperature adjustment, after the atomizing of still top, enter (with propylene oxide reaction) the still, be deposited at the bottom of the still again; Like this circulating reaction, 130～140 ℃ of control reaction temperature, pressure is less than 0.35Mpa, and the add-on of propylene oxide is 11.6 kilograms, after adding, till 130～140 ℃ of insulation reaction no longer descended to the still internal pressure more than 20 minutes; Be cooled to 80～90 ℃;
Second step, the reactor of the first step is vacuumized, under the condition of negative pressure, suck 0.2 kilogram of 50% sodium hydroxide solution as catalyzer, inflated with nitrogen is replaced the air in the still again, the limit vacuumizes, heat up in the limit, and temperature reaches 130～140 ℃, stops heating, guarantee the pumpdown time more than 30 minutes, the stop pumping vacuum; Add minor amount of propylene oxide from the still top-spray, treat that still pushes back backwardness, spraying adds propylene oxide again, along with the adding of propylene oxide, material reaction, temperature in the still progressively raises naturally, the still internal pressure increases, and material is extracted out at the bottom of still by canned-motor pump in the still, after canned-motor pump pressurization, interchanger temperature adjustment, after the atomizing of still top, enter (with propylene oxide reaction) the still, be deposited at the bottom of the still again; Like this circulating reaction, 130～140 ℃ of control reaction temperature, pressure is less than 0.35Mpa, and the add-on of propylene oxide is 82.7 kilograms, after adding, till 130～140 ℃ of insulation reaction no longer descended to the still internal pressure more than 20 minutes; Be cooled to 50～60 ℃, stop canned-motor pump, discharging.Can obtain described allyl amine polyethenoxy ether.
Embodiment five: allyl amine polyoxyethylene poly-oxygen propylene aether (mixing embedding), and its preparation method is as follows:
The first step under negative pressure, drop into 5.7 kilograms allyl amine in the outer circulation of clean exsiccant 200L atomizing still, starts canned-motor pump, and the air in the inflated with nitrogen displacement still below the temperature adjustment to 20 ℃, vacuumizes; Guarantee the pumpdown time more than 30 minutes, the stop pumping vacuum; Slowly material is heated to 130～140 ℃, stop heating, (the mole proportioning of oxyethane and propylene oxide is 1:1 to add the mixture of a small amount of oxyethane and propylene oxide from the reactor top-spray, down together), treat that still pushes back backwardness, spraying adds the mixture of oxyethane and propylene oxide again, adding along with epoxy alkane, temperature in the material reaction, still progressively raises naturally, and the still internal pressure increases; Material is extracted out at the bottom of still by canned-motor pump in the still, after canned-motor pump pressurization, interchanger temperature adjustment, enters after the atomizing of still top (with the epoxy alkane reaction) the still, is deposited at the bottom of the still again; Circulating reaction like this, 130～150 ℃ of control reaction temperature, pressure are less than 0.35Mpa, and the add-on of the mixture of oxyethane and propylene oxide is 10.2 kilograms altogether, after adding, till 130～150 ℃ of insulation reaction no longer descended to the still internal pressure more than 20 minutes; Be cooled to 80～90 ℃;
Second step, the reactor of the first step is vacuumized, under the condition of negative pressure, suck 0.2 kilogram of 50% sodium hydroxide solution as catalyzer, inflated with nitrogen is replaced the air in the still again, the limit vacuumizes, heat up in the limit, and temperature reaches 130～140 ℃, stops heating, guarantee the pumpdown time more than 30 minutes, the stop pumping vacuum; Add the mixture of a small amount of oxyethane and propylene oxide from the reactor top-spray, treat that still pushes back backwardness, spraying adds the mixture of oxyethane and propylene oxide again, adding along with epoxy alkane, temperature in the material reaction, still progressively raises naturally, and the still internal pressure increases.Material is extracted out at the bottom of still by canned-motor pump in the still, after canned-motor pump pressurization, interchanger temperature adjustment, enters after the atomizing of still top (with the epoxy alkane reaction) the still, is deposited at the bottom of the still again; Circulating reaction like this, 130～150 ℃ of control reaction temperature, pressure are less than 0.35Mpa, and the add-on of the mixture of oxyethane and propylene oxide is 84.1 kilograms altogether, after adding, till 130～150 ℃ of insulation reaction no longer descended to the still internal pressure more than 20 minutes; Be cooled to 50～60 ℃, stop canned-motor pump, discharging.Can obtain described allyl amine polyoxyethylene poly-oxygen propylene aether (mixing embedding).
Embodiment six:
Allyl amine polyoxyethylene poly-oxygen propylene aether (block), its preparation method is as follows:
The first step under negative pressure, drop into 5.7 kilograms allyl amine in the outer circulation of clean exsiccant 200L atomizing still, starts canned-motor pump, and the air in the inflated with nitrogen displacement still below the temperature adjustment to 20 ℃, vacuumizes; Guarantee the pumpdown time more than 30 minutes, the stop pumping vacuum; Slowly material is heated to 130～140 ℃, stops heating, add a small amount of oxyethane from the still top-spray, treat that still pushes back backwardness, spraying adds oxyethane again, along with the adding of oxyethane, material reaction, temperature in the still progressively raises naturally, the still internal pressure increases, and material is extracted out at the bottom of still by canned-motor pump in the still, after canned-motor pump pressurization, interchanger temperature adjustment, after the atomizing of still top, enter (with reacting ethylene oxide) the still, be deposited at the bottom of the still again; Like this circulating reaction, 160～170 ℃ of control reaction temperature, pressure is less than 0.35Mpa, and the add-on of oxyethane is 8.8 kilograms altogether, after adding, till 160～170 ℃ of insulation reaction no longer descended to the still internal pressure more than 20 minutes; Be cooled to 80～90 ℃;
Second step, the reactor of the first step is vacuumized, under the condition of negative pressure, suck 0.3 kilogram of 50% sodium hydroxide solution as catalyzer, inflated with nitrogen is replaced the air in the still again, the limit vacuumizes, heat up in the limit, and temperature reaches 130～140 ℃, stops heating, guarantee the pumpdown time more than 30 minutes, the stop pumping vacuum; Add minor amount of propylene oxide from the still top-spray, treat that still pushes back backwardness, spraying adds propylene oxide again, and along with the adding of propylene oxide, material reaction is accelerated, temperature in the still progressively raises naturally, the still internal pressure increases, and material is extracted out at the bottom of still by canned-motor pump in the still, after canned-motor pump pressurization, interchanger temperature adjustment, after the atomizing of still top, enter (with propylene oxide reaction) the still, be deposited at the bottom of the still again; So the circulating reaction control reaction temperature is 130～140 ℃, and pressure is less than 0.35Mpa, and the add-on of propylene oxide is 23.2 kilograms altogether, after adding, till 130～140 ℃ of insulation reaction no longer descended to the still internal pressure more than 30 minutes; Spraying adds oxyethane again,, 160～170 ℃ of control reaction temperature, pressure is less than 0.35Mpa, and the add-on of oxyethane is 62.3 kilograms altogether, after adding, till 160～170 ℃ of insulation reaction no longer descended to the still internal pressure more than 20 minutes; Be cooled to 50～60 ℃, stop canned-motor pump, discharging.Can obtain described allyl amine polyoxyethylene poly-oxygen propylene aether (block).
With the allyl amine polyethers that the foregoing description four to six obtains, respectively its color and luster, total amine value and tertiary amine value are measured result such as following table:
The determination data of table 2 allyl amine polyethers
As can be seen from the above table, the product color that the present invention obtains is good, and total amine value and tertiary amine value difference are little.
Claims (7)
1. an alkenyl amine polyethers is characterized in that, adopts following structural to express:
Wherein, R
1Thiazolinyl for carbonatoms 3～6; M, n, p and q are the integer more than or equal to 0, and m and n be not 0 simultaneously, and p and q are not 0 simultaneously.
2. the preparation method of the described alkenyl amine polyethers of claim 1 is characterized in that, comprises the steps:
(1) under negative pressure, in reactor, add alkenyl amine, start outer circulation, behind the air in the inflated with nitrogen replacement reaction kettle, below the temperature adjustment to 20 ℃, vacuumize then, again material in reactor is heated to 130～140 ℃ after, add epoxy alkane and also carry out circulating reaction, temperature of reaction is 130～170 ℃, reaction pressure is less than 0.4MPa, adds the back 130～170 ℃ of following insulation reaction at least 20 minutes, and cooling is cooled to 80～90 ℃ again; Wherein, the mol ratio of alkenyl amine and epoxy alkane is 1:2～1:4;
(2) aforesaid reaction vessel is vacuumized after, suck catalyzer, the air in the inflated with nitrogen replacement reaction kettle again, vacuumize, be heated to 130～140 ℃, add epoxy alkane then and carry out circulating reaction, temperature of reaction is 130～170 ℃, reaction pressure is less than 0.4MPa, add the back till 130～170 ℃ of following insulation reaction at least 20 minutes no longer descend to reacting kettle inner pressure, cooling is cooled to 50～60 ℃ again, stops outer circulation, discharging promptly obtains described alkenyl amine polyethers; Wherein, the mol ratio of alkenyl amine and epoxy alkane is 1:9～1:66;
Wherein, catalyzer is sodium hydroxide solution or methanol solution of sodium methylate described in the step (2).
3. the preparation method of alkenyl amine polyethers according to claim 2 is characterized in that: the alkenyl amine in the described step (1) and the mol ratio of epoxy alkane are 1:2.
4. the preparation method of alkenyl amine polyethers according to claim 2 is characterized in that: before adding the epoxy alkane reactant, add a small amount of epoxy alkane earlier and carry out pre-reaction in described step (1) and the step (2).
5. the preparation method of alkenyl amine polyethers according to claim 2 is characterized in that: the epoxy alkane that adds in the described step (1) is an oxyethane, and its addition reaction temperature is 160～170 ℃.
6. the preparation method of alkenyl amine polyethers according to claim 2 is characterized in that: the epoxy alkane that adds in the described step (1) is a propylene oxide, and its addition reaction temperature is 130～140 ℃.
7. the preparation method of alkenyl amine polyethers according to claim 2 is characterized in that: the epoxy alkane that adds in the described step (1) is the mixture of oxyethane and propylene oxide, and its addition reaction temperature is 130～150 ℃.
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| CN102219895A (en) * | 2011-06-10 | 2011-10-19 | 海安县国力化工有限公司 | Allylamine polyoxyethylene and its preparation method |
| CN102268133A (en) * | 2011-06-10 | 2011-12-07 | 海安县国力化工有限公司 | Allyl amine polyoxyethylene polyoxypropylene ether and preparation method thereof |
| CN102219895B (en) * | 2011-06-10 | 2012-11-21 | 海安县国力化工有限公司 | Allylamine polyoxyethylene and its preparation method |
| CN103254420A (en) * | 2011-12-28 | 2013-08-21 | 辽宁奥克化学股份有限公司 | Low molecular weight polyether water reducing agent, its preparation method and application |
| CN103755946A (en) * | 2013-12-26 | 2014-04-30 | 四川石达化学股份有限公司 | Double-branch allylamine polyethenoxy ether and synthetic method thereof |
| CN103804677A (en) * | 2014-02-21 | 2014-05-21 | 山东昊达化学有限公司 | Dialkylene amine polyether and preparation method and application thereof |
| CN104262603A (en) * | 2014-10-10 | 2015-01-07 | 天津工业大学 | Polyether demulsifier taking polyether amine as initiator and preparation method of polyether demulsifier |
| CN109681177A (en) * | 2017-10-18 | 2019-04-26 | 中国石油化工股份有限公司 | Using the method for foam discharging agent composition liquid discharging gas producing |
| CN109681177B (en) * | 2017-10-18 | 2021-09-03 | 中国石油化工股份有限公司 | Method for discharging liquid and producing gas by adopting foam discharging agent composition |
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| CN101367928B (en) | 2011-01-26 |
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