CN105968061A - Preparation method of trimethylol melamine - Google Patents
Preparation method of trimethylol melamine Download PDFInfo
- Publication number
- CN105968061A CN105968061A CN201610465621.6A CN201610465621A CN105968061A CN 105968061 A CN105968061 A CN 105968061A CN 201610465621 A CN201610465621 A CN 201610465621A CN 105968061 A CN105968061 A CN 105968061A
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- CN
- China
- Prior art keywords
- preparation
- melamine
- formaldehyde
- trimethylol melamine
- tripolycyanamide
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D251/00—Heterocyclic compounds containing 1,3,5-triazine rings
- C07D251/02—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
- C07D251/12—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members
- C07D251/26—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members with only hetero atoms directly attached to ring carbon atoms
- C07D251/40—Nitrogen atoms
- C07D251/54—Three nitrogen atoms
- C07D251/64—Condensation products of melamine with aldehydes; Derivatives thereof
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Phenolic Resins Or Amino Resins (AREA)
Abstract
The invention discloses a preparation method of trimethylol melamine. The preparation method comprises the following steps: feeding a formaldehyde solution into a reaction kettle according to a mole ratio of melamine : formaldehyde : water of 1:(2.5-3.5):(8-30), and adding water and melamine in sequence for reaction by adjusting temperature and rotating speed. Compared with the conventional process, the preparation method has the advantages that the synthesis process is simple, and raw materials are readily available and easy to separate and purify; due to the reduction of raw material components, the production cost of trimethylol melamine is greatly reduced, the conversion rate of melamine is increased, and the formaldehyde content is reduced; meanwhile, resources are also saved, production of wastewater is reduced, and the environment is protected.
Description
Technical field
The present invention relates to the field of chemical synthesis, be specifically related to the preparation method of a kind of trimethylol melamine.
Background technology
Trimethylol melamine is commonly used for as fabrics for shrinkage, crease proofing agent, make fabric well-pressed, plentiful,
Keep away dirt；This product can prepare melamine resin, can be used for paper and fabric finishing agent；This product
Imino group etherificate product amino resin can also be prepared with alcohols reaction, extensively be used as textile resins finishing agent,
Cross-linking agent, the field such as water-proofing agent.Trimethylol melamine is mainly by tripolycyanamide at present, three ethanol
Amine or methanol and formaldehyde reaction obtain, but due to addition sequence, addition, component and technological parameter
Difference, the waste water of the method generation and by-product are many or react insufficient, and then cause the conversion of tripolycyanamide
Rate is low, and Formaldehyde In Wastewarter is big, reclaims tripolycyanamide and formaldehyde, then increases into product cost.As specially
Profit number is Chinese invention patent " the production work of a kind of hexakis(hydroxymethyl)melamine of 201010561762.0
Skill ", disclose a kind of hexakis(hydroxymethyl)melamine production technology, including batch mixing, reactive crystallization, be centrifuged and divide
From steps such as, evaporations, this technique need to be by solving wastewater problem with formaldehyde plant coproduction.With hexamethylol
Tripolycyanamide is compared, and trimethylol melamine dissolubility in water is relatively big, and more being dissolved in of product reacts residual
Liquid, is not readily separated, and loss is relatively big, and containing formaldehyde, difficult treatment in waste water, production cost is the highest, because of
This this kind of technique is the most rare.
Summary of the invention
In order to solve above-mentioned deficiency and defect, the present invention proposes one can improve tripolycyanamide conversion ratio
The preparation method of trimethylol melamine.
To achieve these goals, the present invention is achieved through the following technical solutions:
The preparation method of a kind of trimethylol melamine, comprises the following steps:
(1) by tripolycyanamide: formaldehyde: water mol ratio is 1: (2.5-3.5): (8-30) is to reactor
The formalin of the above-mentioned metering of middle input, regulation reactor rotating speed is 40-150 rev/min, adds above-mentioned meter
The water of amount, adds alkali regulation pH value and adds the three of above-mentioned metering to 7.0-11.0, regulation temperature after being 25-50 DEG C
Poly cyanamid, is warming up to 30-75 DEG C after stirring 10-30min, and whole process alkali keeps pH to be 7.0-11.0；
(2) treating that tripolycyanamide is completely dissolved, regulation reactor mixing speed is 50-80 rev/min, reaction
1-3h；
(3) stop stirring, stand crystallize 1-3h, centrifugation, slough waste water, be drying to obtain finished product three hydroxyl
Methyl melamine, products obtained therefrom is white particle or powder.
Preferably, tripolycyanamide described in step (1): formaldehyde: your ratio of hydromassage is 1: 2.5: 8.
Preferably, alkali described in step (1) is any one in sodium carbonate, potassium carbonate and sodium hydroxide.
Preferably, described in step (1), alkali is sodium hydroxide.
Preferably, described formaldehyde is the formalin of mass fraction 35%～55%.
Preferably, described in step (1), pH refers to as 7.0-9.0.
The preparation method of trimethylol melamine of the present invention, it has the beneficial effects that: compared with traditional handicraft,
Synthesis technique is simple, raw material is easy to get, isolated and purified easily, the minimizing of raw material components greatly reduces three hydroxyl first
The production cost of base tripolycyanamide, improves the conversion ratio of tripolycyanamide, reduces content of formaldehyde, also saves simultaneously
About resource, decreases the generation of waste water, protects environment.
Detailed description of the invention
Further describe the present invention below in conjunction with specific embodiment, the most simply apply specific case
Principle and embodiment to the embodiment of the present invention are set forth, and are only applicable to help and understand that the present invention is real
Execute the principle of example；Simultaneously for one of ordinary skill in the art, according to the embodiment of the present invention, specifically
All will change on embodiment and range of application, in sum, this specification content should not be understood
For limitation of the present invention.
Embodiment 1
The preparation method of a kind of trimethylol melamine, comprises the following steps:
(1) by tripolycyanamide: formaldehyde: water mol ratio is to reactor in put into above-mentioned metering at 1: 3: 30
Formalin, in formalin, content of formaldehyde is 40%, regulation reactor rotating speed be 50 revs/min, add
The water of above-mentioned metering, adds alkali regulation pH value to 8.0, and regulation temperature adds the trimerization of above-mentioned metering after being 40 DEG C
Cyanamide, is warming up to 50 DEG C after stirring 30min, and whole process sodium hydroxide solution keeps pH to be 8.0；
(2) treating that tripolycyanamide is completely dissolved, reduce reactor mixing speed, regulation converter is 60 revs/min
Clock, reacts 2h；
(3) stop stirring, stand crystallize 3h, centrifugation, slough waste water, be drying to obtain finished product three hydroxyl first
Base tripolycyanamide, products obtained therefrom is white particle or powder, and conversion ratio is 70% (in terms of tripolycyanamide).
Embodiment 2
The preparation method of a kind of trimethylol melamine, comprises the following steps:
(1) by tripolycyanamide: formaldehyde: water mol ratio is to reactor in put into above-mentioned based at 1: 3.5: 20
The formalin of amount, in formalin, content of formaldehyde is 40%, and regulation reactor rotating speed is 100 revs/min,
Add the water of above-mentioned metering, add alkali regulation pH value to 8.0, regulation temperature be 40 DEG C after add above-mentioned metering
Tripolycyanamide, is warming up to 50 DEG C after stirring 30min, and whole process with 30% wet chemical holding pH is
9.0；
(2) treating that tripolycyanamide is completely dissolved, reduce reactor mixing speed, regulation converter is 90 revs/min
Clock, reacts 4h；
(3) stop stirring, stand crystallize 3h, centrifugation, slough waste water, be drying to obtain finished product three hydroxyl first
Base tripolycyanamide, products obtained therefrom is white particle or powder, and conversion ratio is 65% (in terms of tripolycyanamide).
Embodiment 3
The preparation method of a kind of trimethylol melamine, comprises the following steps:
(1) by tripolycyanamide: formaldehyde: water mol ratio is to reactor in put into above-mentioned metering at 1: 2.5: 8
Formalin, in formalin, content of formaldehyde is 40%, regulation reactor rotating speed be 80 revs/min, add
The water of above-mentioned metering, adds alkali regulation pH value to 7.0, and regulation temperature adds the trimerization of above-mentioned metering after being 40 DEG C
Cyanamide, is warming up to 50 DEG C after stirring 30min, and whole process keeps pH to be 7.0 with 30% wet chemical；
(2) treating that tripolycyanamide is completely dissolved, reduce reactor mixing speed, regulation converter is 90 revs/min
Clock, reacts 4h；
(3) stop stirring, stand crystallize 3h, centrifugation, slough waste water, be drying to obtain finished product three hydroxyl first
Base tripolycyanamide, products obtained therefrom is white particle or powder, and conversion ratio is 73% (in terms of tripolycyanamide).
Embodiment 4
The preparation method of a kind of trimethylol melamine, comprises the following steps:
(1) by tripolycyanamide: formaldehyde: water mol ratio is to reactor in put into above-mentioned metering at 1: 2.5: 8
Formalin, in formalin, content of formaldehyde is 40%, regulation reactor rotating speed be 50 revs/min, add
The water of above-mentioned metering, adds alkali regulation pH value to 8.0, and regulation temperature adds the trimerization of above-mentioned metering after being 40 DEG C
Cyanamide, is warming up to 50 DEG C after stirring 30min, and whole process keeps pH to be 9.0 with 30% wet chemical；
(2) treating that tripolycyanamide is completely dissolved, reduce reactor mixing speed, regulation converter is 60 revs/min
Clock, reacts 4h；
(3) stop stirring, stand crystallize 3h, centrifugation, slough waste water, be drying to obtain finished product three hydroxyl first
Base tripolycyanamide, products obtained therefrom is white particle or powder, and conversion ratio is 75% (in terms of tripolycyanamide).
Claims (6)
1. the preparation method of a trimethylol melamine, it is characterised in that: comprise the following steps:
(1) by tripolycyanamide: formaldehyde: water mol ratio is 1: (2.5-3.5): (8-30) is to reactor
The formalin of the above-mentioned metering of middle input, regulation reactor rotating speed is 40-150 rev/min, adds above-mentioned meter
The water of amount, adds alkali regulation pH value and adds the three of above-mentioned metering to 7.0-11.0, regulation temperature after being 25-50 DEG C
Poly cyanamid, is warming up to 30-75 DEG C after stirring 10-30min, and whole process alkali keeps pH to be 7.0-11.0；
(2) treating that tripolycyanamide is completely dissolved, regulation reactor mixing speed is 50-80 rev/min, reaction
1-3h；
(3) stop stirring, stand crystallize 1-3h, centrifugation, slough waste water, be drying to obtain finished product three hydroxyl
Methyl melamine, products obtained therefrom is white particle or powder.
The preparation method of trimethylol melamine the most according to claim 1, it is characterised in that:
Tripolycyanamide described in step (1): formaldehyde: your ratio of hydromassage is 1: 2.5: 8.
The preparation method of trimethylol melamine the most according to claim 1, it is characterised in that:
Alkali described in step (1) is any one in sodium carbonate, potassium carbonate and sodium hydroxide.
The preparation method of trimethylol melamine the most according to claim 1, it is characterised in that:
Described in step (1), alkali is sodium hydroxide.
The preparation method of trimethylol melamine the most according to claim 1, it is characterised in that:
Described formaldehyde is the formalin of mass fraction 35%～55%.
The preparation method of trimethylol melamine the most according to claim 1, it is characterised in that:
Described in step (1), pH refers to as 7.0-9.0.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610465621.6A CN105968061A (en) | 2016-06-23 | 2016-06-23 | Preparation method of trimethylol melamine |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610465621.6A CN105968061A (en) | 2016-06-23 | 2016-06-23 | Preparation method of trimethylol melamine |
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| CN105968061A true CN105968061A (en) | 2016-09-28 |
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| CN201610465621.6A Pending CN105968061A (en) | 2016-06-23 | 2016-06-23 | Preparation method of trimethylol melamine |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110028383A (en) * | 2019-04-23 | 2019-07-19 | 上海大学 | The separation method of polyol mixture by-product |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103881076A (en) * | 2014-03-07 | 2014-06-25 | 济南大学 | Halogen-free hyper-branched intumescent flame retardant and preparation method thereof |
-
2016
- 2016-06-23 CN CN201610465621.6A patent/CN105968061A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103881076A (en) * | 2014-03-07 | 2014-06-25 | 济南大学 | Halogen-free hyper-branched intumescent flame retardant and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| XUE JIAO LIU，ET AL.: "Highly stretchable and tough double network hydrogels via molecular stent", 《EUROPEAN POLYMER JOURNAL》 * |
| YAJUNWANG，ET AL.: "Trifunctional cross-linker trimethylol melamine enhancing adhesiveforce of PVA hydrogels", 《J.APPL.POLYM.SCI.》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110028383A (en) * | 2019-04-23 | 2019-07-19 | 上海大学 | The separation method of polyol mixture by-product |
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Application publication date: 20160928 |