CN102219895B - Allylamine polyoxyethylene and its preparation method - Google Patents
Allylamine polyoxyethylene and its preparation method Download PDFInfo
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- CN102219895B CN102219895B CN2011101548132A CN201110154813A CN102219895B CN 102219895 B CN102219895 B CN 102219895B CN 2011101548132 A CN2011101548132 A CN 2011101548132A CN 201110154813 A CN201110154813 A CN 201110154813A CN 102219895 B CN102219895 B CN 102219895B
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Abstract
The invention provides allylamine polyoxyethylene and its preparation method. The structural formula of allylamine polyoxyethylene provided in the present invention is: CH2=CH-CH2-N-(H)[(C2H4O)nH], wherein, n is an integer no less than 2. According to the method for preparing allylamine polyoxyethylene, allylamine and oxirane are taken as raw materials, and pure water is taken as a solvent. The invention has the following advantages: 1. the obtained allylamine polyoxyethylene has a single branched structure and good color, which can be taken as a raw material to one-step synthesize a high performance polycarboxylate dispersant; 2. the invention employs a combination of an outer circulation atomization reactor and a solvent of water, which has creativity; 3. the invention has the advantages of simple preparation method, reliable technology, stable and safe reaction, and is capable of obtaining the aim objects for one step without using a catalyst.
Description
Technical field
The present invention relates to a kind of polyethers, specifically, relate to a kind of allyl amine Soxylat A 25-7 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 polycarboxylate salt dispersant more economically.
Summary of the invention
The objective of the invention is to overcome the weak point of prior art, a kind of allyl amine Soxylat A 25-7 and preparation method thereof is provided.
Allyl amine Soxylat A 25-7 of the present invention is characterized in that, its structural formula is following:
CH
2=CH-CH
2-N-(H)[(C
2H
4O)
nH]
Wherein, n is not less than 2 integer.
C
2H
4O is an oxyethylene group.This target compound mainly has single branched structure.
The method for preparing the allyl amine Soxylat A 25-7 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 carry out addition reaction; Temperature of reaction is 90～110 ℃, and reaction pressure is less than 0.3Mpa, add required oxyethane 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 is 1: (2～100).
Preferably, described pure water add-on is allyl amine and oxyethane quality sum.
Before adding the reacting ethylene oxide thing, add a small amount of oxyethane earlier and carry out pre-reaction.
The addition reaction temperature that adds oxyethane is 95～105 ℃.
Allyl amine Soxylat A 25-7 of the present invention mainly as raw material with acrylic monomer synthesized high-performance polycarboxylate salt dispersant.
Compared with prior art, the present invention has following advantage:
1. the allyl amine Soxylat A 25-7 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 polycarboxylate salt dispersant.
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 Soxylat A 25-7 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 a small amount of oxyethane, treat that still pushes back backwardness, continue to add oxyethane again, along with the adding of oxyethane, the 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, and after canned-motor pump pressurization, interchanger temperature adjustment, the atomizing back gets into the still (with reacting ethylene oxide) from the still top, is deposited at the bottom of the still again; Like this circulating reaction, 95～105 ℃ of control reaction temperature, pressure is less than 0.30Mpa, and the add-on of oxyethane is 88 kilograms altogether, after adding, till 95～105 ℃ 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 Soxylat A 25-7.
Embodiment 2
Allyl amine Soxylat A 25-7 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 a small amount of oxyethane, treat that still pushes back backwardness; Continue again to add oxyethane, along with the adding of oxyethane, material reaction; Temperature natural in the still progressively raises, and 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, the atomizing back gets into the still (with reacting ethylene oxide) from the still top, is deposited at the bottom of the still again; Like this circulating reaction, 95～105 ℃ of control reaction temperature, pressure is less than 0.30Mpa, and the add-on of oxyethane is 88 kilograms altogether, after adding, till 95～105 ℃ 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 Soxylat A 25-7.
Embodiment 3
Allyl amine Soxylat A 25-7 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 a small amount of oxyethane, treat that still pushes back backwardness; Continue again to add oxyethane, along with the adding of oxyethane, material reaction; Temperature natural in the still progressively raises, and 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, the atomizing back gets into the still (with reacting ethylene oxide) from the still top, is deposited at the bottom of the still again; Like this circulating reaction, 95～105 ℃ of control reaction temperature, pressure is less than 0.30Mpa, and the add-on of oxyethane is 92.4 kilograms altogether, after adding, till 95～105 ℃ 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 Soxylat A 25-7.
Embodiment 4
With the allyl amine Soxylat A 25-7 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 the product of single branched structure that reaction generates is many.
Claims (4)
1. the method for preparing the allyl amine Soxylat A 25-7, said allyl amine Soxylat A 25-7 structural formula is following:
CH
2=CH-CH
2-NH-[(C
2H
4O)
nH]
Wherein, n is not less than 2 integer,
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 carry out addition reaction; Temperature of reaction is 90～110 ℃, and reaction pressure is less than 0.3Mpa, add required oxyethane 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 is 1: (2～100).
2. the preparation method of allyl amine Soxylat A 25-7 according to claim 1 is characterized in that, described pure water add-on is allyl amine and oxyethane quality sum.
3. the preparation method of allyl amine Soxylat A 25-7 according to claim 1 is characterized in that, before adding the reacting ethylene oxide thing, adds a small amount of oxyethane earlier and carries out pre-reaction.
4. the preparation method of allyl amine Soxylat A 25-7 according to claim 1 is characterized in that, the addition reaction temperature that adds oxyethane is 95～105 ℃.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101548132A CN102219895B (en) | 2011-06-10 | 2011-06-10 | Allylamine polyoxyethylene and its preparation method |
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|---|---|---|---|
| CN2011101548132A CN102219895B (en) | 2011-06-10 | 2011-06-10 | Allylamine polyoxyethylene and its preparation method |
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| CN102219895A CN102219895A (en) | 2011-10-19 |
| CN102219895B true CN102219895B (en) | 2012-11-21 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103951798A (en) * | 2014-04-01 | 2014-07-30 | 海安县国力化工有限公司 | Polycarboxylate dispersant and its preparation method |
| 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 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000265095A (en) * | 1999-03-12 | 2000-09-26 | Seiko Epson Corp | Ink composition |
| CN101367928A (en) * | 2008-09-12 | 2009-02-18 | 苏州弗克新型建材有限公司 | Alkene based amine polyether and method of preparing the same |
-
2011
- 2011-06-10 CN CN2011101548132A patent/CN102219895B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000265095A (en) * | 1999-03-12 | 2000-09-26 | Seiko Epson Corp | Ink composition |
| CN101367928A (en) * | 2008-09-12 | 2009-02-18 | 苏州弗克新型建材有限公司 | Alkene based amine polyether and method of preparing the same |
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