CN104829798A - Preparation method of highly methylated amino resin - Google Patents
Preparation method of highly methylated amino resin Download PDFInfo
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- CN104829798A CN104829798A CN201510180085.0A CN201510180085A CN104829798A CN 104829798 A CN104829798 A CN 104829798A CN 201510180085 A CN201510180085 A CN 201510180085A CN 104829798 A CN104829798 A CN 104829798A
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- 229920003180 amino resin Polymers 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 title abstract 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 105
- YGCOKJWKWLYHTG-UHFFFAOYSA-N [[4,6-bis[bis(hydroxymethyl)amino]-1,3,5-triazin-2-yl]-(hydroxymethyl)amino]methanol Chemical compound OCN(CO)C1=NC(N(CO)CO)=NC(N(CO)CO)=N1 YGCOKJWKWLYHTG-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000010792 warming Methods 0.000 claims description 30
- 238000009413 insulation Methods 0.000 claims description 20
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 15
- 238000004821 distillation Methods 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 11
- 239000010455 vermiculite Substances 0.000 claims description 9
- 229910052902 vermiculite Inorganic materials 0.000 claims description 9
- 235000019354 vermiculite Nutrition 0.000 claims description 9
- 239000003513 alkali Substances 0.000 claims description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- IOVCWXUNBOPUCH-UHFFFAOYSA-N Nitrous acid Chemical compound ON=O IOVCWXUNBOPUCH-UHFFFAOYSA-N 0.000 claims description 5
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 claims description 5
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 5
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 5
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- ZXGIFJXRQHZCGJ-UHFFFAOYSA-N erbium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Er+3].[Er+3] ZXGIFJXRQHZCGJ-UHFFFAOYSA-N 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- 229940071870 hydroiodic acid Drugs 0.000 claims description 2
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 2
- MMKQUGHLEMYQSG-UHFFFAOYSA-N oxygen(2-);praseodymium(3+) Chemical compound [O-2].[O-2].[O-2].[Pr+3].[Pr+3] MMKQUGHLEMYQSG-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 9
- 238000005265 energy consumption Methods 0.000 abstract description 7
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 230000018044 dehydration Effects 0.000 abstract 1
- 238000006297 dehydration reaction Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 238000003541 multi-stage reaction Methods 0.000 abstract 1
- 238000007254 oxidation reaction Methods 0.000 description 6
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 5
- 230000009466 transformation Effects 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 description 2
- 229920000877 Melamine resin Polymers 0.000 description 2
- 239000004640 Melamine resin Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 229910052691 Erbium Inorganic materials 0.000 description 1
- 229930040373 Paraformaldehyde Natural products 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 229920002866 paraformaldehyde Polymers 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000002560 therapeutic procedure Methods 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000004634 thermosetting polymer Substances 0.000 description 1
- 238000007039 two-step reaction Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Phenolic Resins Or Amino Resins (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention relates to a preparation method of highly methylated amino resin. The method comprises the following steps: carrying out a multi-step reaction on methanol and hexamethylolmelamine, carrying out normal pressure dealcoholysis, carrying out reduced pressure dehydration, and filtering to obtain the highly methylated amino resin. The preparation method has the advantages of high conversion rate, safe reaction and production, simple process, low energy consumption, simple post-treatment, low cost, small environmental pollution, good product quality and easy condition control.
Description
Technical field
The present invention relates to a kind of preparation method of resin, particularly relate to a kind of good product quality, condition easily controls, the preparation method of height methyl-etherified aminoresin that energy consumption is low.
Background technology
Product amino resin is the thermosetting polymer generated by trimeric cyanamide and formalin or paraformaldehyde polycondensation.Good aminoresin should have the high-performances such as wide, the excellent electrical insulating property of color gamut, flame retardant resistance, high temperature resistant, anti-pollution, water-fast, safety and sanitation.Methyl-etherified aminoresin is widely used in metal preprocessing coating, water-borne coatings and car paint, in general, generating process is by trimeric cyanamide elder generation and formaldehyde reaction, and reacted product reacts with methyl alcohol again, the finished product obtained by a series of subsequent disposal.But this method for making energy consumption is high, and aldehyde-containing sewage is many, and length consuming time, production capacity is low.
In the Chinese invention patent of application number 2012105563846, disclose a kind of preparation method of high imino-methyl-etherified melamine resin, the method passes through two-step reaction, and to the weight ratio between feed composition, addO-on therapy order, time, composition, the adjustment such as procedure reaction parameter, obtain high imino-methyl-etherified melamine resin, its weak point is, this method for making energy consumption is high, and aldehyde-containing sewage is many, length consuming time, production capacity is low.
Summary of the invention
The method energy consumption that the object of the invention is to solve existing preparation high methyl-etherified aminoresin is high, aldehyde-containing sewage is many, length consuming time, the low defect of production capacity and a kind of good product quality is provided, the preparation method of condition easily controls, energy consumption is low height methyl-etherified aminoresin.
To achieve these goals, the present invention is by the following technical solutions:
A preparation method for height methyl-etherified aminoresin, described preparation method comprises the following steps:
A) catalyzer, the methyl alcohol of methyl alcohol total mass 30% and hexamethylolmelamine is added in a kettle., be warming up to 40-48 DEG C, add acid for adjusting pH to 3-4.2, insulation 40-50min, then continue to be warming up to 55-57 DEG C, insulation 2.5-3h, adds alkali and regulates pH to 8.8-9, be warming up to 100-105 DEG C of distillation;
B) step a) is cooled to 45-50 DEG C after completing, and continues the methyl alcohol adding methyl alcohol total mass 50%, adds acid for adjusting pH to 3-4.2, insulation 3-3.5h, adds alkali and regulates pH to 8.8-9, be warming up to 110-115 DEG C of distillation;
C) step b) is cooled to 45-50 DEG C after completing, continue to add remaining methyl alcohol, add acid for adjusting pH to 3-3.8, insulation 30-90min, add alkali and regulate pH to 8.8-9, be warming up to 95-98 DEG C of air distillation 1-2h, then open vacuum system, continue to be warming up to 110 DEG C, continue 3.5-4h, product is squeezed into finished product still, filters and obtain height methyl-etherified aminoresin.
As preferably, the mass ratio of described hexamethylolmelamine and methyl alcohol is 1-2:4.5-5.5.
As preferably, catalyzer is the mixture of yttrium oxide and vermiculite, Erbium trioxide and the mixture of vermiculite or the mixture of Praseodymium trioxide and vermiculite.
As preferably, the add-on of catalyzer is the 3-5.5% of hexamethylolmelamine quality, and in catalyzer, the mass ratio of two kinds of materials is 1:1.
As preferably, described acid is formic acid, hydroiodic acid HI, acid iodide, nitrous acid, sulfurous acid or hypochlorous acid.
As preferably, described alkali is sodium hydroxide, saleratus or sodium bicarbonate.
As preferably, in step c), vacuum tightness is 0.01-0.05MPa.
Beneficial effect of the present invention is that preparation method's transformation efficiency of the present invention is high, reaction production safety, and technique is simple, and energy consumption is low, and aftertreatment is simple, and cost is low, and environmental pollution is little, good product quality, and condition easily controls.
Embodiment
Below in conjunction with specific embodiment, the present invention is further explained:
Embodiment 1
Raw material is hexamethylolmelamine and methyl alcohol, and the mass ratio of hexamethylolmelamine and methyl alcohol is 1:4.5.
A preparation method for height methyl-etherified aminoresin, described preparation method comprises the following steps:
A) mixture of catalyst oxidation yttrium and vermiculite, the methyl alcohol of methyl alcohol total mass 30% and hexamethylolmelamine is added in a kettle., be warming up to 40 DEG C, add first acid for adjusting pH to 3, insulation 40min, then continue to be warming up to 55 DEG C, insulation 2.5h, hydro-oxidation sodium regulates pH to 8.8, is warming up to 100 DEG C of distillations; Wherein, the add-on of catalyzer is the 3-5.5% of hexamethylolmelamine quality;
B) step a) is cooled to 45 DEG C after completing, and continues the methyl alcohol adding methyl alcohol total mass 50%, adds first acid for adjusting pH to 3, insulation 3h, and hydro-oxidation sodium regulates pH to 8.8, is warming up to 110 DEG C of distillations;
C) step b) is cooled to 45 DEG C after completing, continue to add remaining methyl alcohol, add first acid for adjusting pH to 3, insulation 30min, hydro-oxidation sodium regulates pH to 8.8, be warming up to 95 DEG C of air distillation 1h, then open vacuum system, being evacuated to vacuum tightness is 0.01MPa, continue to be warming up to 110 DEG C, continue 3.5h, product is squeezed into finished product still, filter and obtain height methyl-etherified aminoresin.Transformation efficiency is that 92%(is in hexamethylolmelamine).
Embodiment 2
Raw material is hexamethylolmelamine and methyl alcohol, and the mass ratio of hexamethylolmelamine and methyl alcohol is 1.5:5.7.
A preparation method for height methyl-etherified aminoresin, described preparation method comprises the following steps:
A) mixture of catalyst oxidation erbium and vermiculite, the methyl alcohol of methyl alcohol total mass 30% and hexamethylolmelamine is added in a kettle., be warming up to 45 DEG C, add sulfurous acid for adjusting pH to 3.5, insulation 45min, then continue to be warming up to 56 DEG C, insulation 2.7h, adds saleratus and regulates pH to 8.9, be warming up to 103 DEG C of distillations; Wherein, the add-on of catalyzer is 4% of hexamethylolmelamine quality;
B) step a) is cooled to 48 DEG C after completing, and continues the methyl alcohol adding methyl alcohol total mass 50%, adds sulfurous acid for adjusting pH to 3.5, insulation 3.2h, adds saleratus and regulates pH to 8.9, be warming up to 112 DEG C of distillations;
C) step b) is cooled to 48 DEG C after completing, continue to add remaining methyl alcohol, add sulfurous acid for adjusting pH to 3.5, insulation 60min, add saleratus and regulate pH to 8.9, be warming up to 97 DEG C of air distillation 1.5h, then open vacuum system, being evacuated to vacuum tightness is 0.03MPa, continue to be warming up to 110 DEG C, continue 3.8h, product is squeezed into finished product still, filter and obtain height methyl-etherified aminoresin.Transformation efficiency is that 93%(is in hexamethylolmelamine).
Embodiment 3
Raw material is hexamethylolmelamine and methyl alcohol, and the mass ratio of hexamethylolmelamine and methyl alcohol is 2:5.5.
A preparation method for height methyl-etherified aminoresin, described preparation method comprises the following steps:
A) mixture of catalyst oxidation praseodymium and vermiculite, the methyl alcohol of methyl alcohol total mass 30% and hexamethylolmelamine is added in a kettle., be warming up to 48 DEG C, add nitrous acid for adjusting pH to 4.2, insulation 50min, then continue to be warming up to 57 DEG C, insulation 3h, adds sodium bicarbonate and regulates pH to 9, be warming up to 105 DEG C of distillations; Wherein, the add-on of catalyzer is 5.5% of hexamethylolmelamine quality;
B) step a) is cooled to 50 DEG C after completing, and continues the methyl alcohol adding methyl alcohol total mass 50%, adds nitrous acid for adjusting pH to 4.2, insulation 3.5h, adds sodium bicarbonate and regulates pH to 9, be warming up to 115 DEG C of distillations;
C) step b) is cooled to 50 DEG C after completing, continue to add remaining methyl alcohol, add nitrous acid for adjusting pH to 3.8, insulation 90min, add sodium bicarbonate and regulate pH to 9, be warming up to 98 DEG C of air distillation 2h, then open vacuum system, being evacuated to vacuum tightness is 0.05MPa, continue to be warming up to 110 DEG C, continue 4h, product is squeezed into finished product still, filter and obtain height methyl-etherified aminoresin.Transformation efficiency is that 95%(is in hexamethylolmelamine).
Claims (7)
1. a preparation method for height methyl-etherified aminoresin, it is characterized in that, described preparation method comprises the following steps:
A) catalyzer, the methyl alcohol of methyl alcohol total mass 30% and hexamethylolmelamine is added in a kettle., be warming up to 40-48 DEG C, add acid for adjusting pH to 3-4.2, insulation 40-50min, then continue to be warming up to 55-57 DEG C, insulation 2.5-3h, adds alkali and regulates pH to 8.8-9, be warming up to 100-105 DEG C of distillation;
B) step a) is cooled to 45-50 DEG C after completing, and continues the methyl alcohol adding methyl alcohol total mass 50%, adds acid for adjusting pH to 3-4.2, insulation 3-3.5h, adds alkali and regulates pH to 8.8-9, be warming up to 110-115 DEG C of distillation;
C) step b) is cooled to 45-50 DEG C after completing, continue to add remaining methyl alcohol, add acid for adjusting pH to 3-3.8, insulation 30-90min, add alkali and regulate pH to 8.8-9, be warming up to 95-98 DEG C of air distillation 1-2h, then open vacuum system, continue to be warming up to 110 DEG C, continue 3.5-4h, product is squeezed into finished product still, filters and obtain height methyl-etherified aminoresin.
2. the preparation method of a kind of height methyl-etherified aminoresin according to claim 1, is characterized in that, the mass ratio of described hexamethylolmelamine and methyl alcohol is 1-2:4.5-5.5.
3. the preparation method of a kind of height methyl-etherified aminoresin according to claim 1, is characterized in that, catalyzer is the mixture of yttrium oxide and vermiculite, Erbium trioxide and the mixture of vermiculite or the mixture of Praseodymium trioxide and vermiculite.
4. the preparation method of a kind of height methyl-etherified aminoresin according to claim 1 or 3, it is characterized in that, the add-on of catalyzer is the 3-5.5% of hexamethylolmelamine quality, and in catalyzer, the mass ratio of two kinds of materials is 1:1.
5. the preparation method of a kind of height methyl-etherified aminoresin according to claim 1 or 2 or 3, it is characterized in that, described acid is formic acid, hydroiodic acid HI, acid iodide, nitrous acid, sulfurous acid or hypochlorous acid.
6. the preparation method of a kind of height methyl-etherified aminoresin according to claim 1 or 2 or 3, it is characterized in that, described alkali is sodium hydroxide, saleratus or sodium bicarbonate.
7. the preparation method of a kind of height methyl-etherified aminoresin according to claim 1 or 2 or 3, it is characterized in that, in step c), vacuum tightness is 0.01-0.05MPa.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105585684A (en) * | 2016-01-12 | 2016-05-18 | 浙江新华新材料科技有限责任公司 | Method and equipment for preparing full-water-soluble high-imino partial-methylated amino resin |
| CN106279590A (en) * | 2016-08-01 | 2017-01-04 | 浙江新华新材料科技有限责任公司 | Mixed etherified amino resins intumescent rigid foam plastic fire retardant preparation method and reactor |
| CN106750075A (en) * | 2016-12-08 | 2017-05-31 | 浙江亚迪纳新材料科技股份有限公司 | A kind of low preparation technology for gluing methyl etherified Lauxite of high stability |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101817913A (en) * | 2010-03-11 | 2010-09-01 | 浙江奥仕化学有限公司 | Preparation method of highly methyl etherified amino resin |
| CN103709353A (en) * | 2013-12-14 | 2014-04-09 | 山东沾化奥仕化学有限公司 | High-hydroxyl methylated melamine resin and preparation method thereof |
| 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 |
-
2015
- 2015-04-16 CN CN201510180085.0A patent/CN104829798B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101817913A (en) * | 2010-03-11 | 2010-09-01 | 浙江奥仕化学有限公司 | Preparation method of highly methyl etherified amino resin |
| CN103709353A (en) * | 2013-12-14 | 2014-04-09 | 山东沾化奥仕化学有限公司 | High-hydroxyl methylated melamine resin and preparation method thereof |
| 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 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105585684A (en) * | 2016-01-12 | 2016-05-18 | 浙江新华新材料科技有限责任公司 | Method and equipment for preparing full-water-soluble high-imino partial-methylated amino resin |
| CN106279590A (en) * | 2016-08-01 | 2017-01-04 | 浙江新华新材料科技有限责任公司 | Mixed etherified amino resins intumescent rigid foam plastic fire retardant preparation method and reactor |
| CN106750075A (en) * | 2016-12-08 | 2017-05-31 | 浙江亚迪纳新材料科技股份有限公司 | A kind of low preparation technology for gluing methyl etherified Lauxite of high stability |
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