CN102268133B - Allyl amine polyoxyethylene polyoxypropylene ether and preparation method thereof - Google Patents
Allyl amine polyoxyethylene polyoxypropylene ether and preparation method thereof Download PDFInfo
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- CN102268133B CN102268133B CN2011101547801A CN201110154780A CN102268133B CN 102268133 B CN102268133 B CN 102268133B CN 2011101547801 A CN2011101547801 A CN 2011101547801A CN 201110154780 A CN201110154780 A CN 201110154780A CN 102268133 B CN102268133 B CN 102268133B
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- allyl amine
- oxyethane
- propylene oxide
- amine polyoxyethylene
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Abstract
The invention provides allyl amine polyoxyethylene polyoxypropylene ether and a preparation method thereof. The structural formula of allyl amine polyoxyethylene polyoxypropylene ether is CH2=CH-CH2-N-(H)[(C3H6O)m(C2H4O)nH], wherein m and n are integers not less than 2. In the preparation method of allyl amine polyoxyethylene polyoxypropylene ether, allylamine, ethylene oxide and propylene oxide are used as raw materials and pure water is used as a solvent. The invention has the following advantages that: 1. the obtained allyl amine polyoxyethylene polyoxypropylene ether has a single-branched structure and good color, and can be used as a raw material for synthesizing a polycarboxylate dispersant with high performance and a defoaming function in one step; 2. a creative method combining an external circulating aerosol reactor and the solvent (water) is used; and 3. the preparation method provided by the invention has simple and reliable process and stable and safe reaction, and can be used for preparing the target by one-step reaction without use of a catalyst.
Description
Technical field
The present invention relates to a kind of polyethers, specifically, relate to a kind of allyl amine polyoxyethylene poly-oxygen propylene aether and preparation method thereof, belong to technical field of organic chemistry.
Background technology
Improving constantly of Along with people's standard of living, people propose increasingly high requirement to living environment, and high-grade paint is essential, and this just needs the excellent dispersion agent of dispersing property.The raw material that necessary for this reason exploitation makes new advances can prepare high-performance more economically and have the polycarboxylate dispersant who presses down the bubble function.
Summary of the invention
The objective of the invention is to overcome the weak point of prior art, a kind of allyl amine polyoxyethylene poly-oxygen propylene aether and preparation method thereof is provided.
Allyl amine polyoxyethylene poly-oxygen propylene aether of the present invention, structural formula is following:
CH
2=CH-CH
2-N-(H)[(C
3H
6O)
m(C
2H
4O)
nH]
Wherein, m, n are not less than 2 integer.
The method for preparing the allyl amine polyoxyethylene poly-oxygen propylene aether of the present invention comprises the steps: under negative pressure, outwards drops into allyl amine and pure water in the circulating reaction still; Behind the air in the inflated with nitrogen replacement reaction kettle, start the outer circulation pump, below the temperature adjustment to 20 ℃; Vacuumize then and remove remnant oxygen, again material in reactor is heated to 90～95 ℃ afterwards after, slowly add oxyethane and propylene oxide and carry out addition reaction; Temperature of reaction is 90～110 ℃, and reaction pressure is less than 0.3Mpa, add required oxyethane, propylene oxide after; 90～110 ℃ of following insulation reaction at least 30 minutes, cooling was cooled to 40～50 ℃ again; Wherein, the mol ratio of allyl amine and oxyethane, propylene oxide is 1: (2～100): (2～10).
Among the preparation method of described allyl amine polyoxyethylene poly-oxygen propylene aether, the pure water add-on is allyl amine, oxyethane and propylene oxide quality sum.The addition reaction temperature that adds oxyethane, propylene oxide is 90～100 ℃.The adding mode of oxyethane and propylene oxide adds for mixing.The mole number of the oxyethane that adds is more than propylene oxide.
Allyl amine polyoxyethylene poly-oxygen propylene aether of the present invention has the polycarboxylate dispersant who presses down the bubble function mainly as raw material with the acrylic monomer synthesized high-performance.
Compared with prior art, the present invention has following advantage:
1. the allyl amine polyoxyethylene poly-oxygen propylene aether of the present invention's acquisition has single branched structure, and color and luster is good, can be used as raw material one-step synthesis high-performance and has the polycarboxylate dispersant who presses down the bubble function.
2. in the preparing method's of the present invention step, adopt outer circulation atomizing reactor drum and solvent---water bonded method, creative.
3. preparation method of the present invention is simple, and technology is reliable, and reacting balance safety only needs a step can obtain target compound without catalyzer.
Embodiment
Below in conjunction with embodiment the present invention is further described, but should not limit protection scope of the present invention with this:
Embodiment 1
Allyl amine polyoxyethylene poly-oxygen propylene aether in the present embodiment, its preparation method is following:
Under negative pressure, in the outer circulation of clean exsiccant 250L atomizing reaction kettle, drop into 11.4 kilograms allyl amine and 99.4 kilograms pure water, the air in the inflated with nitrogen displacement still starts canned-motor pump, below the temperature adjustment to 20 ℃, vacuumizes; Guarantee the pumpdown time more than 30 minutes, the stop pumping vacuum; Slowly material is heated to 90～95 ℃, stops heating, in reaction kettle, add the mixture of a small amount of oxyethane, propylene oxide; Treat that still pushes back backwardness; Continue again to add oxyethane, propylene oxide, along with the adding of oxyethane, propylene oxide mixture, material reaction; Temperature natural in the still progressively raises, and the still internal pressure increases; Material is extracted out at the bottom of still by canned-motor pump in the still, and after canned-motor pump pressurization, interchanger temperature adjustment, the atomizing back gets into the still (with oxyethane, propylene oxide reaction) from the still top, is deposited at the bottom of the still again; Circulating reaction like this, 90～100 ℃ of control reaction temperature, pressure is less than 0.30Mpa, and the add-on of oxyethane, propylene oxide is 88 kilograms altogether, and wherein the add-on of propylene oxide is 23.2 kilograms.After adding, till 90～100 ℃ of insulation reaction no longer descended to the still internal pressure more than 30 minutes; Be cooled to 40～50 ℃, stop canned-motor pump, discharging.Can obtain said allyl amine polyoxyethylene poly-oxygen propylene aether.
Embodiment 2
Allyl amine polyoxyethylene poly-oxygen propylene aether in the present embodiment; Its preparation method is following: under negative pressure, in the outer circulation of clean exsiccant 250L atomizing reaction kettle, drop into 5.7 kilograms allyl amine and 93.7 kilograms pure water; Air in the inflated with nitrogen displacement still; Start canned-motor pump, below the temperature adjustment to 20 ℃, vacuumize; Guarantee the pumpdown time more than 30 minutes, the stop pumping vacuum; Slowly material is heated to 90～95 ℃, stops heating, in reaction kettle, add the mixture of a small amount of oxyethane, propylene oxide; Treat that still pushes back backwardness, continue to add the mixture of oxyethane, propylene oxide again, along with the adding of oxyethane, propylene oxide mixture; Temperature natural in the material reaction, still progressively raises, 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, the atomizing back gets into the still (with oxyethane, propylene oxide reaction) from the still top, is deposited at the bottom of the still again; Circulating reaction like this, 90～100 ℃ of control reaction temperature, pressure is less than 0.30Mpa, and the add-on of oxyethane, propylene oxide is 88 kilograms altogether, and wherein the add-on of propylene oxide is 17.4 kilograms.After adding, till 90～100 ℃ of insulation reaction no longer descended to the still internal pressure more than 30 minutes; Be cooled to 40～50 ℃; Stop canned-motor pump, discharging.Can obtain said allyl amine polyoxyethylene poly-oxygen propylene aether.
Embodiment 3
Allyl amine polyoxyethylene poly-oxygen propylene aether in the present embodiment; Its preparation method is following: under negative pressure, in the outer circulation of clean exsiccant 250L atomizing reaction kettle, drop into 3.99 kilograms allyl amine and 96.39 kilograms pure water; Air in the inflated with nitrogen displacement still; Start canned-motor pump, below the temperature adjustment to 20 ℃, vacuumize; Guarantee the pumpdown time more than 30 minutes, the stop pumping vacuum; Slowly material is heated to 90～95 ℃, stops heating, in reaction kettle, add the mixture of a small amount of oxyethane, propylene oxide; Treat that still pushes back backwardness, continue to add the mixture of oxyethane, propylene oxide again, along with the adding of oxyethane, propylene oxide mixture; Temperature natural in the material reaction, still progressively raises, 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, the atomizing back gets into the still (with oxyethane, propylene oxide reaction) from the still top, is deposited at the bottom of the still again; Circulating reaction like this, 90～100 ℃ of control reaction temperature, pressure is less than 0.30Mpa, and the add-on of oxyethane, propylene oxide is 92.4 kilograms altogether, and wherein the add-on of propylene oxide is 16.24 kilograms.After adding, till 90～100 ℃ of insulation reaction no longer descended to the still internal pressure more than 30 minutes; Be cooled to 40～50 ℃; Stop canned-motor pump, discharging.Can obtain said allyl amine polyoxyethylene poly-oxygen propylene aether.
Embodiment 4
With the allyl amine polyoxyethylene poly-oxygen propylene aether that the foregoing description 1 to 3 obtains, respectively its color and luster, total amine value and tertiary amine value are measured result such as following table:
Can find out that from last table the product color that the present invention obtains is good; Tertiary amine value is little, explains that reaction has generated the product of single branched structure.
Claims (6)
1. an allyl amine polyoxyethylene poly-oxygen propylene aether is characterized in that, its structural formula is following:
CH
2=CH-CH
2-NH[(C
3H
6O)
m(C
2H
4O)
nH]
Wherein, m, n are not less than 2 integer.
2. prepare the method for the described allyl amine polyoxyethylene poly-oxygen propylene aether of claim 1, it is characterized in that, comprise the steps: under negative pressure; Outwards drop into allyl amine and pure water in the circulating reaction still, behind the air in the inflated with nitrogen replacement reaction kettle, start the outer circulation pump; Below the temperature adjustment to 20 ℃, vacuumize then and remove remnant oxygen, again material in reactor is heated to 90～95 ℃ afterwards after; Slowly add oxyethane and propylene oxide and carry out addition reaction, temperature of reaction is 90～110 ℃, and reaction pressure is less than 0.3Mpa; After adding required oxyethane, propylene oxide, 90～110 ℃ of following insulation reaction at least 30 minutes, cooling was cooled to 40～50 ℃ again; Wherein, the mol ratio of allyl amine and oxyethane, propylene oxide is 1: (2～100): (2～10).
3. the preparation method of allyl amine polyoxyethylene poly-oxygen propylene aether according to claim 2 is characterized in that, described pure water add-on is allyl amine, oxyethane and propylene oxide quality sum.
4. the preparation method of allyl amine polyoxyethylene poly-oxygen propylene aether according to claim 2 is characterized in that, the addition reaction temperature that adds oxyethane, propylene oxide is 90～100 ℃.
5. the preparation method of allyl amine polyoxyethylene poly-oxygen propylene aether according to claim 2 is characterized in that, the adding mode of oxyethane and propylene oxide adds for mixing.
6. the preparation method of allyl amine polyoxyethylene poly-oxygen propylene aether according to claim 2 is characterized in that, the mole number of the oxyethane of adding is more than propylene oxide.
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| CN103951794A (en) * | 2014-04-01 | 2014-07-30 | 海安县国力化工有限公司 | Low-foam polycarboxylate dispersant and its preparation method |
| CN104084086B (en) * | 2014-07-17 | 2016-01-13 | 天津悦泰石化科技有限公司 | For the surfactant and its production and use of urea for vehicle solution |
| CN105482095A (en) * | 2015-12-22 | 2016-04-13 | 南京红宝丽聚氨酯有限公司 | Unsaturated polyether alcohol and polycarboxylate water reducer prepared by same |
| CN111234202B (en) * | 2020-02-27 | 2022-10-04 | 中科院广州化学有限公司 | Solvent-free high-nitrogen-content polycarboxyl type hyperdispersant as well as preparation method and application thereof |
| CN113372507A (en) * | 2020-09-15 | 2021-09-10 | 吉林奥克新材料有限公司 | Cross-linking polyether ester amide water reducing agent and preparation method thereof |
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Effective date of registration: 20180530 Address after: 276400 Shandong Linyi Yishui Yishui Economic Development Zone Mount Lu project area fine chemical industrial park Changshan Guan Zhuang Village South Patentee after: LINYI GUOLI CHEMICAL Co.,Ltd. Address before: 226600 Nanhai Road (middle) 19, Chengdong Town, Haian County, Nantong, Jiangsu Patentee before: HAI'AN GUOLI CHEMICAL Co.,Ltd. |
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Denomination of invention: Allylamine polyoxyethylene polyoxypropylene ether and its preparation method Effective date of registration: 20230907 Granted publication date: 20120725 Pledgee: Postal Savings Bank of China Limited Yishui County sub branch Pledgor: LINYI GUOLI CHEMICAL Co.,Ltd. Registration number: Y2023980055681 |