CN107353379B - High butylated amino resin is synthesized using trimethylol melamine - Google Patents
High butylated amino resin is synthesized using trimethylol melamine Download PDFInfo
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- CN107353379B CN107353379B CN201710825827.XA CN201710825827A CN107353379B CN 107353379 B CN107353379 B CN 107353379B CN 201710825827 A CN201710825827 A CN 201710825827A CN 107353379 B CN107353379 B CN 107353379B
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- kettle
- air inlet
- reaction kettle
- isobutanol
- trimethylol melamine
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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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- Phenolic Resins Or Amino Resins (AREA)
Abstract
High butylated amino resin is synthesized using trimethylol melamine, comprising: successively puts into isobutanol and trimethylol melamine in proportion into reaction kettle；It controls temperature and adds acid for adjusting pH value；It is passed through ammonia after reaction and adjusts pH value；Dimethylbenzene is added and carries out normal pressure dealcoholysis, dehydration；Temperature is controlled again and carries out vacuum dehydration processing；And cooling filtering.Present invention obtains the high butylated amino resins of function admirable, significantly reduce wastewater treatment capacity, and reduce production cost.
Description
Technical field
The present invention relates to the environmental protection synthesis of high butylated amino resin.
Background technique
Etherified amino resins are synthesized using melamine such as hexamethylolmelamine or tetra methylol melamine etc.,
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 that the etherified resin of flame-retardant composition is introduced by hydridization.But above-mentioned synthesis
Method causes very burden due to needing using a large amount of lye, to subsequent water process, increases treatment process and cost,
And it is unfavorable for environment protection emission.In addition, metal ion contained in lye also subsequent filter is caused it is unfavorable.
Summary of the invention
The object of the present invention is to provide a kind of synthetic methods of high butylated amino resin, can at least overcome above-mentioned existing
Certain defect for thering is technology to refer to.
The synthetic method of high butylated amino resin according to the present invention includes:
Isobutanol is put into reaction kettle；
Adjusting reactor agitator revolving speed is 60~100 revs/min, and is to slowly warm up to 70~105 DEG C；
Acid adding adjusts in kettle solution ph to 3.0~6.0；
Reactor agitator revolving speed is reduced to be 30~50 revs/min and trimethylol melamine is added into reaction kettle,
Wherein trimethylol melamine: the molar ratio of isobutanol is 1: (5~20)；
1~3h of insulation reaction；
Ammonia is passed through reaction kettle, adjusts in kettle pH value of solution to 8~9；
Be added isobutanol amount 5%~15% dimethylbenzene, be gradually warming up to 100 DEG C of progresss normal pressure dealcoholysis, be dehydrated 30~
60min；
1~3h is handled to solution vacuum dehydration in kettle at 105~115 DEG C of temperature；And
Gained colourless viscous liquid is high butylated amino resin after cooling filtering.
It according to a particular embodiment of the invention, can also include viscosity-adjusting agent step, medium viscosity before cooling filtering
It is adjusted to 2000~6000mPa.s.
Preferred embodiment in accordance with the present invention can be equipped with multiple aeration heads being connected to ammonia pipe, institute in reaction kettle
Stating aeration head includes the ontology with central symmetry axis and the central symmetry axis installation air inlet on the body perpendicular to ontology
Straight tube, ontology have the semi-spherical portion in central cylindrical portion and centrally located cylindrical portion either side, and the top dome end of semi-spherical portion opens up aeration
Hole opens up air inlet in the circumferential wall in central cylindrical portion, and wherein air inlet is connect 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 equipped with multilayer aeration head in a kettle.Every layer may include to
Few two aeration heads.The distance between adjacent layer is incremented by upwards from reactor bottom.This arrangement is very beneficial for ammonia
Quickly be passed through and spread.In addition, the diameter of solarization air cap (or gas 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 vertically to mutually stagger.
Aeration head design according to the present invention, ammonia substantially tangentially enters inside aeration head simultaneously therefore can be along inner peripheral wall
High speed is circled round, and from two sides solarization air cap high speed ejection and therefore can be readily entered sticky molten along central symmetry axis later
Liquid, and form nanoscale microbubble and be quickly mixed into viscosity solution (forming ammonium hydroxide).
In a specific embodiment of the present invention, the acid can be hydrochloric acid, sulfuric acid or benzene sulfonic acid, preferably hydrochloric acid.
Synthetic method according to the present invention can synthesize not due to using trimethylol melamine as raw material
With for example sticky more excellent high butylated amino resin of performance.
In addition and it is very crucial, since the invention avoids use lye and take the method for being passed through ammonia to adjust
PH value, therefore wastewater treatment capacity is significantly reduced, to keep synthetic method of the invention 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 design, so that ammonia dissolves in the mistake that viscosity solution forms ammonium hydroxide
Cheng Jiqi is abundant rapidly, to further improve combined coefficient.
Detailed description of the invention
Fig. 1 is the arrangement schematic diagram of the ammonia access equipment in reaction kettle of the invention；And
Fig. 2 is the structural schematic diagram of ammonia aeration head of the invention.
Specific embodiment
The present invention is further illustrated combined with specific embodiments below, it will be understood by those skilled in the art that being described below
Embodiment be intended merely to more fully understand and implement the present invention, not be used to any restrictions are made to the present invention.
Fig. 1 and Fig. 2 diagrammatically illustrates ammonia access equipment and its aeration head in reaction kettle of the invention.
Referring to Fig. 1,1 center of inside location arrangements multilayer aeration head 3 of reaction kettle, the distance between adjacent layer is from reaction kettle bottom
Portion is incremented by upwards.Ammonia supplies each aeration head 3 by pipeline 2.Pipeline 2 and its connected aeration head 3 be inserted into can be convenient or
Take out reaction kettle 1.
Referring to fig. 2, aeration head 3 includes ontology with central symmetry axis (being horizontally through solarization air cap 34 in figure) and vertical
Air inlet straight tube 31 on the body is installed in the central symmetry axis of ontology.Ontology has central cylindrical portion 33 and centrally located cylinder
Portion's either side or the semi-spherical portion of two 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 inlet 32 is opened up, air inlet 32 is connect with air inlet straight tube 31, the inner circle of the circumferential wall in central cylindrical portion 33 at air inlet 32
Perimeter surface is general tangential with airintake direction.
Embodiment 1
Using trimethylol melamine as the high imino group of Material synthesis, high butylated amino resin:
(1) isobutanol is put into reaction kettle, adjusting reactor agitator revolving speed is 60 revs/min, and is to slowly warm up to
80℃；
(2) with 36% hydrochloric acid adjust kettle in solution ph be 3, reduce reactor agitator revolving speed be 30 revs/min simultaneously
Trimethylol melamine is added into reaction kettle, wherein trimethylol melamine: the molar ratio of isobutanol is 1: 8, heat preservation
React 1h；
(3) ammonia is passed through reaction kettle by above-mentioned ammonia access equipment, detecting and adjusting pH value of solution in kettle is 8；
(4) dimethylbenzene of isobutanol amount 8% (mass ratio) is added, is gradually warming up to 100 DEG C of progress normal pressure dealcoholysis, dehydration
30min；
(5) to solution vacuum (vacuum degree 0.09MPa) dehydration 1h in kettle at 105 DEG C of temperature；And
(6) adjusting viscosity is 3000mPa.s, and gained colourless viscous liquid is high butyl ether after cooling (to room temperature) filtering
Amino resins.
Embodiment 2
For step with embodiment 1, difference is as follows:
In step (1), agitator speed is 70 revs/min, is warming up to 90 DEG C；
In step (2), pH value 5,40 revs/min of revolving speed, trimethylol melamine: the molar ratio of isobutanol is 1:
10, insulation reaction 2h；
In step (3), pH value 8.5；
In step (4), the dimethylbenzene of isobutanol amount 10% (mass ratio), normal pressure dealcoholysis, dehydration 50min is added；
In step (5), temperature is 110 DEG C, vacuum degree 0.08MPa, dehydration 2h；
In step (6), adjusting viscosity is 4000mPa.s.
Embodiment 3
For step with embodiment 1, difference is as follows:
In step (1), agitator speed is 100 revs/min, is warming up to 90 DEG C；
In step (2), pH value 5,50 revs/min of revolving speed, trimethylol melamine: the molar ratio of isobutanol is 1:
20, insulation reaction 3h；
In step (3), pH value 9；
In step (4), the dimethylbenzene of isobutanol amount 12% (mass ratio), normal pressure dealcoholysis, dehydration 60min is added；
In step (5), temperature is 110 DEG C, vacuum degree 0.07MPa, dehydration 3h；
In step (6), adjusting viscosity is 5000mPa.s.
Claims (2)
1. a kind of synthetic method of high butylated amino resin, comprising:
Isobutanol is put into reaction kettle；
Adjusting reactor agitator revolving speed is 60~100 revs/min, and is to slowly warm up to 70~105 DEG C；
Acid adding adjusts in kettle solution ph to 3.0~6.0；
Reactor agitator revolving speed is reduced to be 30~50 revs/min and trimethylol melamine is added into reaction kettle, wherein
Trimethylol melamine: the molar ratio of isobutanol is 1: (5~20)；
1~3h of insulation reaction；
Ammonia is passed through reaction kettle, adjusts in kettle pH value of solution to 8~9；
The dimethylbenzene of isobutanol amount 5%~15% is added, is gradually warming up to 100 DEG C of progress normal pressure dealcoholysis, 30~60min of dehydration；
1~3h is handled to solution vacuum dehydration in kettle at 105~115 DEG C of temperature；And
Gained colourless viscous liquid is high butylated amino resin after cooling filtering,
Multiple aeration heads being connected to ammonia pipe are wherein installed, the aeration head includes having central symmetry axis in reaction kettle
Ontology and central symmetry axis installation air inlet straight tube on the body perpendicular to ontology, ontology have central cylindrical portion and are located at
The semi-spherical portion of central cylindrical portion either side, the top dome end of semi-spherical portion open up solarization air cap, opened up in the circumferential wall in central cylindrical portion into
Stomata, wherein air inlet is connect with air inlet straight tube, inner circumferential surface and air inlet in the circumferential wall in air inlet position central cylindrical portion
Direction is general tangential,
The multiple aeration head is the multilayer aeration head for entreating installation in a kettle, and every layer includes at least two aeration heads, adjacent
The distance between layer is incremented by upwards from reactor bottom.
2. synthetic method according to claim 1, wherein further including viscosity-adjusting agent step before cooling filtering, wherein gluing
Degree is adjusted to 2000~6000mPa.s.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710825827.XA CN107353379B (en) | 2017-09-14 | 2017-09-14 | High butylated amino resin is synthesized using trimethylol melamine |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710825827.XA CN107353379B (en) | 2017-09-14 | 2017-09-14 | High butylated amino resin is synthesized using trimethylol melamine |
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| CN107353379A CN107353379A (en) | 2017-11-17 |
| CN107353379B true CN107353379B (en) | 2019-07-12 |
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|---|---|---|---|---|
| CN201010589Y (en) * | 2007-03-05 | 2008-01-23 | 付杰 | Centrifugal aerating head |
| CN102050933A (en) * | 2010-12-17 | 2011-05-11 | 上海涂料有限公司上海新华树脂厂 | Methanol and isobutanol mixed ether amino resin and preparation method thereof |
| CN103709111A (en) * | 2013-12-25 | 2014-04-09 | 重庆建峰浩康化工有限公司 | Synthetic method of etherified 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 |
| CN104562689A (en) * | 2013-10-16 | 2015-04-29 | 圣戈班磨料磨具有限公司 | Backing material treated by amino resin, coated abrasive tool product containing and utilizing backing material as well as preparation method of backing material |
| CN105968282A (en) * | 2016-06-28 | 2016-09-28 | 重庆建峰浩康化工有限公司 | Method for synthesizing high-butyl etherified amino resin by taking hexamethylolmelamine as raw materials |
Family Cites Families (1)
| 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 |
-
2017
- 2017-09-14 CN CN201710825827.XA patent/CN107353379B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201010589Y (en) * | 2007-03-05 | 2008-01-23 | 付杰 | Centrifugal aerating head |
| CN102050933A (en) * | 2010-12-17 | 2011-05-11 | 上海涂料有限公司上海新华树脂厂 | Methanol and isobutanol mixed ether amino resin and preparation method thereof |
| CN104562689A (en) * | 2013-10-16 | 2015-04-29 | 圣戈班磨料磨具有限公司 | Backing material treated by amino resin, coated abrasive tool product containing and utilizing backing material as well as preparation method of backing material |
| CN103709111A (en) * | 2013-12-25 | 2014-04-09 | 重庆建峰浩康化工有限公司 | Synthetic method of etherified 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 |
| CN105968282A (en) * | 2016-06-28 | 2016-09-28 | 重庆建峰浩康化工有限公司 | Method for synthesizing high-butyl etherified amino resin by taking hexamethylolmelamine as raw materials |
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Inventor after: Li Ping Inventor after: Wang Wenwu Inventor after: Hu Jinsong Inventor after: Zhou Jianping Inventor after: Zhang Zhixuan Inventor before: Wang Wenwu Inventor before: Hu Jinsong Inventor before: Zhou Jianping Inventor before: Zhang Zhixuan |
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