CN107353380A - Tetra methylol melamine synthesizes butylated amino resin - Google Patents
Tetra methylol melamine synthesizes butylated amino resin Download PDFInfo
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- CN107353380A CN107353380A CN201710826503.8A CN201710826503A CN107353380A CN 107353380 A CN107353380 A CN 107353380A CN 201710826503 A CN201710826503 A CN 201710826503A CN 107353380 A CN107353380 A CN 107353380A
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- methylol melamine
- tetra methylol
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- 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
- C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08G12/02—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
- C08G12/40—Chemically modified polycondensates
- C08G12/42—Chemically modified polycondensates by etherifying
- C08G12/424—Chemically modified polycondensates by etherifying of polycondensates based on heterocyclic compounds
- C08G12/425—Chemically modified polycondensates by etherifying of polycondensates based on heterocyclic compounds based on triazines
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Organic Chemistry (AREA)
- Phenolic Resins Or Amino Resins (AREA)
Abstract
Tetra methylol melamine synthesizes butylated amino resin, including：Put into butanol and tetra methylol melamine successively in proportion into reactor；Control temperature and add acid for adjusting pH value；Ammonia regulation pH value is passed through after reaction；Add dimethylbenzene and carry out normal pressure dealcoholysis, dehydration；Temperature is controlled again and carries out vacuum dehydration processing；And cooling filtering.Present invention obtains the butylated amino resin of function admirable, significantly reduces wastewater treatment capacity, and reduce production cost.
Description
Technical field
The present invention relates to the environmental protection synthesis of butylated amino resin.
Background technology
Etherified amino resins are synthesized such as hexamethylolmelamine or tetra methylol melamine using melamine,
It may refer to the patent or patent application CN 103739563B, CN 103739803B, CN103709111B, CN before applicant
105968283A, CN105968281A, CN105968282A and CN106008870A.In addition, CN106243300A and
CN106349267A etc. also discloses the synthetic method for the etherified resin that flame-retardant composition is introduced by hydridization.But above-mentioned synthesis
Method causes very burden due to needing to use a large amount of alkali lye, therefore to follow-up water process, increases processing procedure and cost,
And it is unfavorable for environment protection emission.In addition, metal ion contained in alkali lye also subsequent filter is caused it is unfavorable.
The content of the invention
It is an object of the invention to provide a kind of synthetic method of butylated amino resin, and it can at least overcome above-mentioned existing
Certain defect that technology refers to.
Included according to the synthetic method of the butylated amino resin of the present invention：
Butanol is put into reactor；
Solution ph is to 3.0~6.0 in acid adding regulation kettle；
Tetra methylol melamine, wherein tetra methylol melamine are put into reactor again: the mol ratio of butanol is 1
: (5~20)；
Solution in kettle is warming up to 50~90 DEG C；
Regulation reactor stirring frequency converter starts to stir to 10~30Hz, until tetra methylol melamine is completely dissolved；
Solution in kettle is incubated 0.5~2h；
Ammonia is passed through reactor, adjusts in kettle pH value of solution to 8~9；
To solution dealcoholysis dewater treatment 0.5 in kettle under conditions of 60~100 DEG C of temperature and 0.07~0.1MPa of vacuum
~3h, so as to obtain resin first product；
Butanol is added in resin first product so that solid content regulation is between 75%~85%；And
Gained colourless viscous liquid is butylated amino resin after filtering.
According to a particular embodiment of the invention, added butanol can be n-butanol or isobutanol.
According to a preferred embodiment of the invention, multiple aeration heads connected with ammonia pipe, institute can be installed in reactor
State aeration head include with central symmetry axis body and perpendicular to body central symmetry axis be arranged on body on air inlet
Straight tube, body have the semi-spherical portion of central cylindrical portion and centrally located cylindrical portion either side, and the top dome end of semi-spherical portion opens up aeration
Hole, air admission hole is opened up in the circumferential wall in central cylindrical portion, wherein air admission hole is connected with air inlet straight tube, in air inlet position central cylindrical
The inner circumferential surface of the circumferential wall in portion and airintake direction are general tangential.
In the above-described embodiments, further preferably centre is provided with multilayer aeration head in a kettle.Every layer can be included extremely
Few two aeration heads.The distance between adjacent layer is incremented by upwards from reactor bottom.This arrangement is very beneficial for ammonia
Quick be passed through and spread.In addition, the diameter of solarization air cap (or steam vent) is preferably 7-10mm.In addition, the ammonia of each solarization air cap
Gas discharge capacity is preferably 10-12l/m.The aeration head of adjacent layer can also be made mutually to stagger on vertical.
Designed according to the aeration head of the present invention, ammonia substantially tangentially enters simultaneously therefore can be along inner peripheral wall inside aeration head
Circle round at a high speed, it is molten therefore can simultaneously to readily enter viscosity along central symmetry axis from the ejection of both sides solarization air cap high speed afterwards
Liquid, and form nanoscale microbubble and be quickly mixed into viscosity solution (formation ammoniacal liquor).
In a particular embodiment of the present invention, the acid can be hydrochloric acid, sulfuric acid or benzene sulfonic acid, preferably hydrochloric acid.
According to the synthetic method of the present invention, due to using tetra methylol melamine as raw material, therefore can synthesize not
With for example sticky more excellent butylated amino resin of performance.
It is in addition and very crucial, because present invention, avoiding take the method for being passed through ammonia to adjust using alkali lye
PH value, therefore wastewater treatment capacity is significantly reduced, so that the synthetic method of the present invention is very environmentally friendly.Further, since without volume
Outer introducing alkali metal ion, also reduces subsequent filter requirement and cost.
The present invention has also further used efficient aeration head to design so that ammonia dissolves in the mistake that viscosity solution forms ammoniacal liquor
Cheng Jiqi is abundant rapidly, so as to further increase combined coefficient.
Brief description of the drawings
Fig. 1 is the arrangement schematic diagram of the ammonia access equipment in the reactor of the present invention；And
Fig. 2 is the structural representation of the ammonia aeration head of the present invention.
Embodiment
The present invention is further illustrated with reference to specific embodiment, it will be understood by those skilled in the art that description below
Embodiment be intended merely to more fully understand and implement the present invention, not be used for any restrictions are made to the present invention.
Fig. 1 and Fig. 2 diagrammatically illustrates the ammonia access equipment and its aeration head in the reactor of the present invention.
Referring to Fig. 1, the center of inside location arrangements multilayer aeration head 3 of reactor 1, the distance between adjacent layer is from reactor bottom
Portion is incremented by upwards.Ammonia supplies each aeration head 3 by pipeline 2.Pipeline 2 and its connected aeration head 3 can conveniently insert or
Take out reactor 1.
Referring to Fig. 2, aeration head 3 is including the body with central symmetry axis (solarization air cap 34 is horizontally through in figure) and vertically
The air inlet straight tube 31 being arranged in the central symmetry axis of body on body.Body has central cylindrical portion 33 and centrally located cylinder
Portion's either side or the semi-spherical portion of both sides 35.The top dome end of semi-spherical portion 35 opens up solarization air cap 34.In the circumferential wall in central cylindrical portion 33
Air admission hole 32 is opened up, air admission hole 32 is connected with air inlet straight tube 31, the inner circle of the circumferential wall in central cylindrical portion 33 at air admission hole 32
Perimeter surface is general tangential with airintake direction.
Embodiment 1
Using tetra methylol melamine as Material synthesis butylated amino resin：
(1) by tetra methylol melamine: the mol ratio of butanol puts into above-mentioned metering into aforesaid reaction vessel for 1: 20
Butanol, regulation reactor stir frequency converter to 20Hz, add 36% salt acid for adjusting pH value to 3.5, add four hydroxyls of above-mentioned metering
Methyl melamine, heating regulation temperature are that 85 DEG C of stirrings make its dissolving；
(2) after reaction terminates after tetra methylol melamine is completely dissolved, it is incubated 2h；
(3) ammonia is passed through into reactor by above-mentioned ammonia access equipment, detects pH value and adjust pH as 9；
(4) vavuum pump is started, it is 0.08MPa to control vacuum, and temperature is 60 DEG C, dealcoholysis dehydration 3h；
(5) stop vacuumizing, add butanol and adjust solid content to 85%；
(6) colourless viscous liquid product is obtained after filtering.
Embodiment 2
For step with embodiment 1, difference is as follows：
In step (1), tetra methylol melamine: the mol ratio of butanol be 1: 10, regulation reactor stir frequency converter to
30Hz, pH value are adjusted to 5, are warming up to 70 DEG C；
In step (2), 2h is incubated；
In step (3), pH value 8.5；
In step (4), temperature is 80 DEG C, vacuum 0.09MPa, dealcoholysis dewater treatment 2h；
In step (5), solid content is adjusted to 80%.
Embodiment 3
For step with embodiment 1, difference is as follows：
In step (1), tetra methylol melamine: the mol ratio of butanol be 1: 8, regulation reactor stir frequency converter to
10Hz, pH value are adjusted to 6, are warming up to 50 DEG C；
In step (2), 0.5h is incubated；
In step (3), pH value 8；
In step (4), temperature is 100 DEG C, vacuum 0.07MPa, dealcoholysis dewater treatment 0.5h；
In step (5), solid content is adjusted to 75%.
Claims (2)
1. a kind of synthetic method of butylated amino resin, including：
Butanol is put into reactor；
Solution ph is to 3.0~6.0 in acid adding regulation kettle；
Tetra methylol melamine, wherein tetra methylol melamine are put into reactor again: the mol ratio of butanol is 1: (5
~20)；
Solution in kettle is warming up to 50~90 DEG C；
Regulation reactor stirring frequency converter starts to stir to 10~30Hz, until tetra methylol melamine is completely dissolved；
Solution in kettle is incubated 0.5~2h；
Ammonia is passed through reactor, adjusts in kettle pH value of solution to 8~9；
To solution dealcoholysis 0.5~3h of dewater treatment in kettle under conditions of 60~100 DEG C of temperature and 0.07~0.1MPa of vacuum,
So as to obtain resin first product；
Butanol is added in resin first product so that solid content regulation is between 75%~85%；And
Gained colourless viscous liquid is butylated amino resin after filtering.
2. synthetic method according to claim 1, multiple aeration heads connected with ammonia pipe are wherein installed in reactor,
The aeration head includes the body with central symmetry axis and is arranged on entering on body perpendicular to the central symmetry axis of body
Gas straight tube, body have the semi-spherical portion of central cylindrical portion and centrally located cylindrical portion either side, and the top dome end of semi-spherical portion opens up exposure
Stomata, air admission hole is opened up in the circumferential wall in central cylindrical portion, wherein air admission hole is connected with air inlet straight tube, in air inlet position center circle
The inner circumferential surface of the circumferential wall in post portion and airintake direction are general tangential.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710826503.8A CN107353380A (en) | 2017-09-14 | 2017-09-14 | Tetra methylol melamine synthesizes butylated amino resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710826503.8A CN107353380A (en) | 2017-09-14 | 2017-09-14 | Tetra methylol melamine synthesizes butylated amino resin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107353380A true CN107353380A (en) | 2017-11-17 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710826503.8A Withdrawn CN107353380A (en) | 2017-09-14 | 2017-09-14 | Tetra methylol melamine synthesizes butylated amino resin |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60155217A (en) * | 1984-01-24 | 1985-08-15 | Hitachi Chem Co Ltd | Production of butyl-etherified amino resin |
| CN201010589Y (en) * | 2007-03-05 | 2008-01-23 | 付杰 | Centrifugal aerating head |
| CN103739803A (en) * | 2013-12-25 | 2014-04-23 | 重庆建峰浩康化工有限公司 | Synthesis method of imino methylated amino resin |
| CN103739563A (en) * | 2013-12-25 | 2014-04-23 | 重庆建峰浩康化工有限公司 | Synthesis method of imino butylated amino resin |
| CN205275297U (en) * | 2015-12-25 | 2016-06-01 | 山东国环产业投资有限公司 | Spiral -flow aeration ware |
| CN105949417A (en) * | 2016-06-03 | 2016-09-21 | 滁州市龙飞化工有限公司 | Preparation method for butylated melamine-formaldehyde resin |
-
2017
- 2017-09-14 CN CN201710826503.8A patent/CN107353380A/en not_active Withdrawn
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60155217A (en) * | 1984-01-24 | 1985-08-15 | Hitachi Chem Co Ltd | Production of butyl-etherified amino resin |
| CN201010589Y (en) * | 2007-03-05 | 2008-01-23 | 付杰 | Centrifugal aerating head |
| CN103739803A (en) * | 2013-12-25 | 2014-04-23 | 重庆建峰浩康化工有限公司 | Synthesis method of imino methylated amino resin |
| CN103739563A (en) * | 2013-12-25 | 2014-04-23 | 重庆建峰浩康化工有限公司 | Synthesis method of imino butylated amino resin |
| CN205275297U (en) * | 2015-12-25 | 2016-06-01 | 山东国环产业投资有限公司 | Spiral -flow aeration ware |
| CN105949417A (en) * | 2016-06-03 | 2016-09-21 | 滁州市龙飞化工有限公司 | Preparation method for butylated melamine-formaldehyde resin |
Non-Patent Citations (1)
| Title |
|---|
| 彭安顺等: "《精细有机品化学》", 31 August 1996, 石油大学出版社 * |
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Application publication date: 20171117 |