CN107540802A - Pentamethylol melamine synthesizes high Amino resin - Google Patents
Pentamethylol melamine synthesizes high Amino resin Download PDFInfo
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- CN107540802A CN107540802A CN201710970744.XA CN201710970744A CN107540802A CN 107540802 A CN107540802 A CN 107540802A CN 201710970744 A CN201710970744 A CN 201710970744A CN 107540802 A CN107540802 A CN 107540802A
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- pentamethylol melamine
- amino resin
- high amino
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Abstract
Pentamethylol melamine synthesizes high Amino resin, including：Put into methanol and pentamethylol melamine in proportion into reactor；Solution ph in acid adding regulation kettle；Heating stirring is until pentamethylol melamine is completely dissolved；Ammonia is passed through reactor to adjust rise pH；Resin first product is obtained after dealcoholysis dewater treatment；And gained colourless viscous liquid is high Amino resin after filtering.Present invention obtains the special high Amino resin of performance, wastewater treatment capacity is significantly reduced, and reduce production cost.
Description
Technical field
The present invention relates to the environmental protection synthesis of high 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 high Amino resin, and it can at least overcome above-mentioned existing
There is certain defect that technology refers to.
Included according to the synthetic method of the high Amino resin of the present invention：
According to pentamethylol melamine: the mol ratio of methanol is 1: (15~25) first put into methanol into reactor；
Solution ph is to 3.0~5.0 in acid adding regulation kettle；
The pentamethylol melamine of above-mentioned mol ratio is put into reactor again；
Solution in kettle is warming up to 35~55 DEG C；
Regulation reactor stirring frequency converter starts to stir to 10~30Hz, until pentamethylol melamine is completely dissolved；
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；And
Gained colourless viscous liquid is high Amino resin after filtering.
According to a particular embodiment of the invention, filter aid diatomite, added diatomite Functionality, quality and appealing design can also be added during filtering
Elect the 0.5%~1% of pentamethylol melamine quality as.
According to a preferred embodiment of the invention, can also include：After ammonia is passed through, before dealcoholysis dewater treatment, add
Enter 0.1%~0.3% inorganic combustion inhibitor that quality is preferably pentamethylol melamine quality, and at 100 DEG C~130 DEG C
Stirring reaction 30min~60min.Inorganic combustion inhibitor is 1 preferably by mass ratio:1:1 silica, Firebrake ZB and three oxidations two
Antimony forms.The resin of the present invention needs fire-retardant answer by having excellent fire resistance after above-mentioned processing, suitable for various
Use occasion.
According to a preferred embodiment of the invention, reactor internal perisporium can be provided with multiple aerations connected with ammonia pipe
Head, the aeration head include the body with central symmetry axis and are arranged on perpendicular to the central symmetry axis of body on body
Air inlet straight tube, body have the conus portion of central cylindrical portion and centrally located cylindrical portion both sides, and the tapered end of conus portion is opened respectively
If solarization air cap, 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
Entreat inner circumferential surface and the airintake direction of the circumferential wall of cylindrical portion general tangential.
In the above-described embodiments, multilayer aeration head is further preferably installed on reactor internal perisporium.Every layer can wrap
Include 2-6 aeration head.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 pentamethylol melamine as raw material, therefore spy can be synthesized
The high Amino resin of different in nature energy.
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.
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 inwall arranging multiplayer or multi-turn 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.Reactor 1 forms closed container in reaction, prevents ammonia etc.
Effusion.
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
The conus portion of portion both sides.The tapered end of conus portion opens up solarization air cap 34 respectively.Air inlet is opened up in the circumferential wall in central cylindrical portion 33
Hole 32, air admission hole 32 are connected with air inlet straight tube 31, at air admission hole 32 inner circumferential surface of the circumferential wall in central cylindrical portion 33 with
Airintake direction is general tangential.
Embodiment 1
Using pentamethylol melamine as the high Amino resin of Material synthesis：
(1) by pentamethylol melamine: the mol ratio of methanol puts into above-mentioned metering into aforesaid reaction vessel for 1: 20
Methanol, add salt acid for adjusting pH value to 3.5, add the pentamethylol melamine of above-mentioned metering, heating regulation temperature is 55 DEG C and stirred
Mixing (regulation reactor stirs frequency converter to 20Hz) makes its dissolving；
(2) after pentamethylol melamine is completely dissolved, ammonia is passed through into reactor by above-mentioned ammonia access equipment
Gas, detect pH value and adjust pH as 9；
(3) vavuum pump is started, it is 0.08MPa to control vacuum, and temperature is 60 DEG C, dealcoholysis dehydration 3h；
(4) stop vacuumizing, add 0.8% diatomite that quality is pentamethylol melamine quality, stirring
60min；
(5) colourless viscous liquid product is obtained after filtering.
Embodiment 2
For step with embodiment 1, difference is as follows：
In step (1), pentamethylol melamine: the mol ratio of methanol is 1: 15, sulphur acid for adjusting pH value is added to be adjusted to 5.0
Save reactor and stir frequency converter to 30Hz, the regulation temperature that heats up is 45 DEG C and is stirred dissolving；
In step (2), regulation pH value is 8.0；
In step (3), vacuum 0.09MPa is controlled, temperature is 80 DEG C, time 2h；
In step (4), 1% diatomite is added, stirs 90min.
Embodiment 3
For step with embodiment 1, difference is as follows：
In step (1), pentamethylol melamine: the mol ratio of methanol is 1: 25, salt acid for adjusting pH value is added to be adjusted to 4.0
Save reactor and stir frequency converter to 10Hz, the regulation temperature that heats up is 35 DEG C and is stirred dissolving；
In step (2), pH value is adjusted to 8.5；
In step (3), vacuum 0.1MPa is controlled, temperature is 100 DEG C, time 0.5h；
In step (4), 0.6% diatomite is added, stirs 40min.
Embodiment 4
With embodiment 1, difference is step：
Also include step between step (2) and (3)：Add inorganic combustion inhibitor, and the stirring reaction 50min at 110 DEG C.
Inorganic combustion inhibitor by etc. silica, Firebrake ZB and the antimony oxide of parts by weight form, added flame retardant amount is five methylols
The 0.2% of melamine quality.
It should be appreciated by those skilled in the art that above-described embodiment is intended merely to more fully understand and implements the present invention, not
For making any restrictions to the present invention.For example, the step of adding filter aid diatomite can also be omitted in above-described embodiment.
Claims (3)
1. a kind of synthetic method of high Amino resin, including：
According to pentamethylol melamine: the mol ratio of methanol is 1: (15~25) first put into methanol into reactor；
Solution ph is to 3.0~5.0 in acid adding regulation kettle；
The pentamethylol melamine of above-mentioned mol ratio is put into reactor again；
Solution in kettle is warming up to 35~55 DEG C；
Regulation reactor stirring frequency converter starts to stir to 10~30Hz, until pentamethylol melamine is completely dissolved；
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；And
Gained colourless viscous liquid is high Amino resin after filtering.
2. synthetic method according to claim 1, wherein filtration step also include：Add filter aid diatomite, added silicon
Diatomaceous earth quality is the 0.5%~1% of pentamethylol melamine quality.
3. synthetic method according to claim 1, wherein reactor internal perisporium are provided with multiple exposures connected with ammonia pipe
Gas head, the aeration head include the body with central symmetry axis and are arranged on perpendicular to the central symmetry axis of body on body
Air inlet straight tube, body has a conus portion of central cylindrical portion and centrally located cylindrical portion both sides, the tapered end difference of conus portion
Solarization air cap is opened up, 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
The inner circumferential surface of the circumferential wall in central cylindrical portion and airintake direction are general tangential.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710970744.XA CN107540802A (en) | 2017-10-18 | 2017-10-18 | Pentamethylol melamine synthesizes high Amino resin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710970744.XA CN107540802A (en) | 2017-10-18 | 2017-10-18 | Pentamethylol melamine synthesizes high Amino resin |
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| CN107540802A true CN107540802A (en) | 2018-01-05 |
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| CN201710970744.XA Pending CN107540802A (en) | 2017-10-18 | 2017-10-18 | Pentamethylol melamine synthesizes high Amino resin |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108623766A (en) * | 2018-05-23 | 2018-10-09 | 重庆建峰浩康化工有限公司 | The fire-retardant melamine resin of high imino group methyl-etherified and its production method |
| CN108623994A (en) * | 2018-05-23 | 2018-10-09 | 重庆建峰浩康化工有限公司 | The fire-retardant melamine resin of butyl etherization is produced with trimethylol melamine |
| CN110527043A (en) * | 2018-05-23 | 2019-12-03 | 重庆建峰浩康化工有限公司 | The production of the fire-retardant melamine resin of etherization |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108623766A (en) * | 2018-05-23 | 2018-10-09 | 重庆建峰浩康化工有限公司 | The fire-retardant melamine resin of high imino group methyl-etherified and its production method |
| CN108623994A (en) * | 2018-05-23 | 2018-10-09 | 重庆建峰浩康化工有限公司 | The fire-retardant melamine resin of butyl etherization is produced with trimethylol melamine |
| CN110527043A (en) * | 2018-05-23 | 2019-12-03 | 重庆建峰浩康化工有限公司 | The production of the fire-retardant melamine resin of etherization |
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Application publication date: 20180105 |