CN106496482A - The synthesis technique of modified high-solid content melmac - Google Patents
The synthesis technique of modified high-solid content melmac Download PDFInfo
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- CN106496482A CN106496482A CN201611093252.9A CN201611093252A CN106496482A CN 106496482 A CN106496482 A CN 106496482A CN 201611093252 A CN201611093252 A CN 201611093252A CN 106496482 A CN106496482 A CN 106496482A
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- tripolycyanamide
- solid content
- melmac
- modified high
- paraformaldehyde
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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
- C08G12/44—Chemically modified polycondensates by esterifying
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- Phenolic Resins Or Amino Resins (AREA)
Abstract
The present invention relates to resin polymerization new technology, and in particular to a kind of synthesis technique of modified high-solid content melmac.The synthesis technique of described modified high-solid content melmac, comprises the steps：(1) at 80 90 DEG C, polyvinyl alcohol and tripolycyanamide are dissolved in water, add alkali to adjust pH, under the conditions of pH is 8.5 9.0, add paraformaldehyde to be reacted, after reactant liquor clarification, tripolycyanamide and polyformaldehyde reaction is sequentially added, after the clarification of question response liquid, tripolycyanamide and paraformaldehyde is sequentially added, adjust the temperature to 85 DEG C of 1 1.5h of reaction simultaneously, obtain polyhydroxy tripolycyanamide；(2) after adding sodium citrate to react 20 40min, acid for adjusting pH is added to 6.0 6.5, add alcohol and react 1.0 2.0h, obtain modified high-solid content melmac.The present invention reasonable in design, be easily achieved；Obtained modified high-solid content melmac stability is high.
Description
Technical field
The present invention relates to resin polymerization new technology, and in particular to a kind of synthesis work of modified high-solid content melmac
Skill.
Background technology
Tripolycyanamide, calls melamine, also known as man-made protein, is a kind of broad-spectrum basic organic chemical industry intermediate products.
Main purposes is for preparing melmac (abbreviation MF resins).Tripolycyanamide can also make fire retardant, water reducer, first
Aldehyde cleaning agent etc..Tripolycyanamide is a kind of triazines nitrogen heterocyclic ring organic compound, contains a triazine stiffening ring in molecule, because
After this resin solidification, hardness is big, and fragility is high, almost without toughness.Meet high temperature to decompose reaction, a large amount of N can be discharged2, therefore
Good fire resistance is shown, it also has good sound absorption properties, hydrothermal stability, wholesomeness and secondary in addition
Processing characteristics.
Melmac is a kind of traditional amino resins, and melamine resin can be stably made at 150 DEG C
With, and with self-extinguishment, arc resistance and good mechanical property.At present, melamine resin is mainly used in timber and adds
The aspects such as work, molding agent, coating, water reducer, leather finishing agent.But the stability of melmac is with the rising of solid content
And gradually reduce.
Due to common melmac less stable, the final resin stability for obtaining, molecular weight and viscosity pair
Later stage is more notable using affecting.The melmac stability of particularly high solids content is worse, therefore, in synthesis large arch dam
Research is needed to affect the various factors of such performance during amount resin.
Melamine molecule structure contains three active aminos, can generate methylol, most multipotency and 6 with formaldehyde reaction respectively
Molecule formaldehyde reacts hexakis(hydroxymethyl)melamine.But further can be dehydrated between methylol under room temperature, de- formaldehyde condensation anti-
Should.Therefore, MF stable resins are preserved also becomes a hot research problem.At present ripe measure is：It is etherified with alcohols, but
The resins fire retardant performance for obtaining is greatly reduced, and can make powdery MF resins with spray-dried.
The aqueous solution of melamine resin is spray-dried to make powdery MF resins, can solve the storage of MF resins
Problem, but still need to for MF resins to be dissolved in water into solution when melamine formaldehyde resin foam plastics are prepared, due to MF powder in
There is micro microgel particle unavoidably, these microgranules cannot dissolve in course of dissolution, dispersion in aqueous, is preparing foam plastic
Once these microgranules cannot be eliminated during material, these microgranules will cause foam local holes, or even subside.Prepare high solids content
During melamine fat, resin stability is substantially reduced, and easily gel solidification.Therefore search out a suitable method and prepare stable height
Solid content melamine fat has been imperative.
Content of the invention
For the deficiencies in the prior art, it is an object of the invention to provide a kind of conjunction of modified high-solid content melmac
Into technique, reasonable in design, be easily achieved, obtained modified high-solid content melmac stability is high.
The synthesis technique of modified high-solid content melmac of the present invention, comprises the steps：
(1) at 80-90 DEG C, polyvinyl alcohol and tripolycyanamide are dissolved in water, add alkali to adjust pH, be 8.5- in pH
Under the conditions of 9.0, add paraformaldehyde to be reacted, after reactant liquor clarification, sequentially add tripolycyanamide and polyformaldehyde reaction, treat
After reactant liquor clarification, tripolycyanamide and paraformaldehyde is sequentially added, while adjusting the temperature to 85 DEG C of reaction 1-1.5h, obtain polyhydroxy
Base tripolycyanamide；
(2) after adding sodium citrate reaction 20-40min, acid for adjusting pH is added to 6.0-6.5, add alcohol reaction 1.0-
2.0h, obtains modified high-solid content melmac.
Wherein：
In step (1), tripolycyanamide is added three times altogether, adds the tripolycyanamide gross mass of employing for the first time
60%, the 30% of the tripolycyanamide gross mass that second addition is adopted, the tripolycyanamide gross mass that third time addition is adopted
10%.
In step (1), paraformaldehyde is added three times altogether, adds the paraformaldehyde gross mass of employing for the first time
60%, the 30% of the paraformaldehyde gross mass that second addition is adopted, the paraformaldehyde gross mass that third time addition is adopted
10%.
5-8% of the consumption of described polyvinyl alcohol for tripolycyanamide quality.
Described alkali is the sodium hydroxide solution that mass concentration is 10-20%.
In step (1), under the conditions of pH is 8.5, paraformaldehyde is added.
6-7% of the consumption of described sodium citrate for tripolycyanamide quality.
Described acid is hydrochloric acid or organic acid.Organic acid is preferably formic acid or ammonium chloride.
Described alcohol is methanol, isobutanol or ethylene glycol.
The mol ratio of described tripolycyanamide, paraformaldehyde and alcohol is 1：2.2：3, paraformaldehyde is measured with formaldehyde.
Step (2) reaction end is determined by the change of observing response liquid, picks reactant liquor with glass and instill clear water sight
Examine, the change of reactant liquor：Water white transparency is vaporific → and white is vaporific → white drop-wise solid, now as reaction end.
In sum, beneficial effects of the present invention are as follows：
1st, technological design of the present invention rationally, be easily achieved.
2nd, adopt modified high-solid content melmac stability obtained in synthesis technique of the present invention high.
Description of the drawings
Fig. 1 is the synthesis technique figure of modified high-solid content melmac of the present invention.
Specific embodiment
With reference to embodiment, the present invention will be further described.
The raw material adopted in embodiment is commercial.
Embodiment 1
(1) water bath with thermostatic control is warming up to 80 DEG C in advance, measures 120mL distilled water and adds in there-necked flask, adds the poly- second of 6.3g
Enol, adds 75.6g melamine powders, and constant temperature dissolves 15min, adjusts pH=8.5 using 20%NaOH, adds 39.6g
Paraformaldehyde is reacted, and after reactant liquor clarification, sequentially adds 37.8g tripolycyanamide and 19.8g polyformaldehyde reactions, question response
After liquid clarification, 12.6g tripolycyanamide and 6.6g paraformaldehydes is sequentially added, while adjusting the temperature to 85 DEG C of reaction 1.5h, obtained
Polyhydroxy tripolycyanamide；
(2) after adding 7.6g sodium citrates reaction 20min, salt acid for adjusting pH is added to 6.0, add the reaction of 96g methanol
1.0h, obtains modified high-solid content melmac.
Embodiment 2
(1) water bath with thermostatic control is warming up to 85 DEG C in advance, measures 120mL distilled water and adds in there-necked flask, adds the poly- second of 8.1g
Enol, adds 75.6g melamine powders, and constant temperature dissolves 15min, adjusts pH=9.0 using 15%NaOH, adds 39.6g
Paraformaldehyde is reacted, and after reactant liquor clarification, sequentially adds 37.8g tripolycyanamide and 19.8g polyformaldehyde reactions, question response
After liquid clarification, 12.6g tripolycyanamide and 6.6g paraformaldehydes is sequentially added, while 85 DEG C of reaction 1h are adjusted the temperature to, much
Hydroxyl tripolycyanamide；
(2), after adding 8.8g sodium citrates reaction 30min, add first acid for adjusting pH to 6.5, add 186g ethylene glycol anti-
1.5h is answered, modified high-solid content melmac is obtained.
Embodiment 3
(1) water bath with thermostatic control is warming up to 90 DEG C in advance, measures 120mL distilled water and adds in there-necked flask, adds the poly- second of 7.1g
Enol, adds 75.6g melamine powders, and constant temperature dissolves 15min, adjusts pH=8.5 using 10%NaOH, adds 39.6g
Paraformaldehyde is reacted, and after reactant liquor clarification, sequentially adds 37.8g tripolycyanamide and 19.8g polyformaldehyde reactions, question response
After liquid clarification, 12.6g tripolycyanamide and 6.6g paraformaldehydes is sequentially added, while adjusting the temperature to 85 DEG C of reaction 1.2h, obtained
Polyhydroxy tripolycyanamide；
(2), after adding 8.0g sodium citrates reaction 40min, add ammonium chloride pH to be adjusted to 6.5, add 222g isobutanol
Reaction 2.0h, obtains modified high-solid content melmac.
Claims (10)
1. a kind of synthesis technique of modified high-solid content melmac, it is characterised in that：Comprise the steps：
(1) at 80-90 DEG C, polyvinyl alcohol and tripolycyanamide are dissolved in water, add alkali to adjust pH, be 8.5-9.0 in pH
Under the conditions of, add paraformaldehyde to be reacted, after reactant liquor clarification, sequentially add tripolycyanamide and polyformaldehyde reaction, treat anti-
After answering liquid clarification, tripolycyanamide and paraformaldehyde is sequentially added, while adjusting the temperature to 85 DEG C of reaction 1-1.5h, obtain polyhydroxy
Tripolycyanamide；
(2) after adding sodium citrate reaction 20-40min, acid for adjusting pH is added to 6.0-6.5, add alcohol reaction 1.0-2.0h,
Obtain modified high-solid content melmac.
2. the synthesis technique of modified high-solid content melmac according to claim 1, it is characterised in that：Step
(1) in, tripolycyanamide is added three times altogether, adds the 60% of the tripolycyanamide gross mass for adopting for the first time, second addition
Using tripolycyanamide gross mass 30%, third time add adopt tripolycyanamide gross mass 10%.
3. the synthesis technique of modified high-solid content melmac according to claim 1, it is characterised in that：Step
(1) in, paraformaldehyde is added three times altogether, adds the 60% of the paraformaldehyde gross mass for adopting for the first time, second addition
Using paraformaldehyde gross mass 30%, third time add adopt paraformaldehyde gross mass 10%.
4. the synthesis technique of modified high-solid content melmac according to claim 1, it is characterised in that：Described
5-8% of the consumption of polyvinyl alcohol for tripolycyanamide quality.
5. the synthesis technique of modified high-solid content melmac according to claim 1, it is characterised in that：Described
Alkali is the sodium hydroxide solution that mass concentration is 10-20%.
6. the synthesis technique of modified high-solid content melmac according to claim 1, it is characterised in that：Step
(1), in, under the conditions of pH is 8.5, paraformaldehyde is added.
7. the synthesis technique of modified high-solid content melmac according to claim 1, it is characterised in that：Described
6-7% of the consumption of sodium citrate for tripolycyanamide quality.
8. the synthesis technique of modified high-solid content melmac according to claim 1, it is characterised in that：Described
Acid is hydrochloric acid or organic acid.
9. the synthesis technique of modified high-solid content melmac according to claim 1, it is characterised in that：Described
Alcohol is methanol, isobutanol or ethylene glycol.
10. the synthesis technique of modified high-solid content melmac according to claim 1, it is characterised in that：Described
Tripolycyanamide, paraformaldehyde and alcohol mol ratio be 1：2.2：3, paraformaldehyde is measured with formaldehyde.
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| CN201611093252.9A CN106496482A (en) | 2016-11-30 | 2016-11-30 | The synthesis technique of modified high-solid content melmac |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108276540A (en) * | 2018-03-09 | 2018-07-13 | 东北林业大学 | A kind of melamine-urea cocondensation resin and preparation method thereof and a kind of adhesive |
| CN108505391A (en) * | 2018-04-20 | 2018-09-07 | 吴伟华 | A kind of preparation method of high glaze wear-resisting type impregnated paper |
-
2016
- 2016-11-30 CN CN201611093252.9A patent/CN106496482A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108276540A (en) * | 2018-03-09 | 2018-07-13 | 东北林业大学 | A kind of melamine-urea cocondensation resin and preparation method thereof and a kind of adhesive |
| CN108276540B (en) * | 2018-03-09 | 2019-06-11 | 东北林业大学 | A kind of melamine-urea cocondensation resin and preparation method thereof and a kind of adhesive |
| CN108505391A (en) * | 2018-04-20 | 2018-09-07 | 吴伟华 | A kind of preparation method of high glaze wear-resisting type impregnated paper |
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Effective date of registration: 20171017 Address after: Yiyuan County Economic Development Zone 256100 Shandong city of Zibo province (county Yihe Road No. 1329) Applicant after: Shandong Heli Chemical Co., Ltd. Address before: 256100 Yiyuan City, Zibo Province, east wind road, No., No. 36 Applicant before: SHANDONG LIAHERD CHEMICAL INDUSTRY CO., LTD. |
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