CN106349444A - Preparation method of rubber adhesive HMMM (Hexamethoxy Methyl Melamine) - Google Patents
Preparation method of rubber adhesive HMMM (Hexamethoxy Methyl Melamine) Download PDFInfo
- Publication number
- CN106349444A CN106349444A CN201610714987.2A CN201610714987A CN106349444A CN 106349444 A CN106349444 A CN 106349444A CN 201610714987 A CN201610714987 A CN 201610714987A CN 106349444 A CN106349444 A CN 106349444A
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- CN
- China
- Prior art keywords
- minutes
- temperature
- preparation
- methanol
- rubber adhesive
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
-
- 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
- C08G12/427—Melamine
-
- 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
- C08G12/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C08G12/30—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds with substituted triazines
- C08G12/32—Melamines
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J161/00—Adhesives based on condensation polymers of aldehydes or ketones; Adhesives based on derivatives of such polymers
- C09J161/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C09J161/32—Modified amine-aldehyde condensates
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- General Chemical & Material Sciences (AREA)
- Phenolic Resins Or Amino Resins (AREA)
Abstract
The invention relates to a preparation method of a cross-linking agent and in particular relates to a preparation method of a rubber adhesive HMMM (Hexamethoxy Methyl Melamine). After water reacts with paraformaldehyde, methanol is added, and a technological process of etherifying, neutralizing and distilling is carried out. According to the preparation method of the cross-linking agent, an inorganic acid is used as a catalyst and can be used for completely neutralizing; an intermediate product is not generated and the purity of the product is kept.
Description
Technical field
The present invention relates to a kind of preparation method of cross-linking agent, the especially preparation method of rubber adhesive hmmm.
Background technology
Rubber adhesive hmmm, that is, high alkylated melamine (hmmm) is the monomeric compound of 6 degrees of functionality, and outward appearance is pin
Shape crystallizes, 55 DEG C of fusing point, and in water, dissolubility is 10%, dissolves in most of organic solvent, has good heat stability.Technical grade
Hmmm viscosity is low, and the degree of cross linking is high, has with various oil content alkyd resin, polyester resin, thermosetting acrylic resin, epoxy resin
Good compatibility, is applied to solvent-borne type decorative paint, coil coating, powdery paints, can lacquer, high solid coating, water
Property coating is it can also be used to ink industry, paper industry etc..Conventional HMMM resin is with hexamethylol three
Poly cyanamid is reacted with methanol in acid condition, and conventional catalyst is organic acid, because organic acid is not complete when neutralization
Full response, and easy and product generation intermedium.
Content of the invention
For above-mentioned technical problem, the present invention provide a kind of acid can neutralization completely HMMM resin
Production technology, specific technical scheme is:
The preparation method of rubber adhesive hmmm, comprises the following steps:
(1) water, paraformaldehyde are added in a kettle., it is 7～8 that hydro-oxidation sodium adjusts ph value, after stirring, then puts into melamine
Amine, is heated to 40～50 DEG C, is incubated 30 minutes～100 minutes；Adjusting ph value with sodium hydroxide is 8～10, is then heated to 50
～80 DEG C, it is incubated 30 minutes～100 minutes；It is down to 40 DEG C；Adjust ph with sulphuric acid to neutrality；
(2) add methanol in a kettle., under stirring；Reactor begins to warm up, and when temperature reaches 48～58 DEG C, adds sulfur
Acid carries out etherification reaction, and 2～3, temperature keeps constant to ph, after material becomes clear, continues insulation 60～120 minutes；
(3) keeping temperature, adds sodium hydroxide neutralization, and ph reaches 7.5～9.0, and the response time keeps more than 5～10 minutes；
(4) heat temperature raising, makes methanol distill out, and methanol is carried out with cooling recovery；
(5) when temperature reaches 75～85 DEG C, then recovered under reduced pressure, when vacuum is not less than 0.08mpa, 125 DEG C～135 DEG C of temperature
When, stop heating, continue vacuum 60～120 minutes, final temperature keeps 125 DEG C～140 DEG C, regard in cylinder no distillation as
Only, release vacuum, cooling had both obtained hexamethylol melamine resin.
The present invention provide rubber adhesive hmmm preparation method, mineral acid is used as catalyst, can completely in
With, and intermediate product will not be produced, keep the purity of product.
Specific embodiment
It is described in conjunction with the embodiments the specific embodiment of the present invention.
(1) water, paraformaldehyde are added in a kettle., it is 7～8 that hydro-oxidation sodium adjusts ph value, after stirring, then puts into three
Poly cyanamid, is heated to 40～50 DEG C, is incubated 30 minutes～100 minutes；Adjusting ph value with sodium hydroxide is 8～10, then heats
To 50～80 DEG C, it is incubated 30 minutes～100 minutes；It is down to 40 DEG C；Adjust ph with sulphuric acid to neutrality；
(2) add methanol in a kettle., under stirring, reactor begins to warm up, when temperature reaches 48～58 DEG C, add sulfur
Acid carries out etherification reaction, and 2～3, temperature keeps constant to ph, after material becomes clear, continues insulation 60～120 minutes；
(3) keeping temperature, adds sodium hydroxide neutralization, and ph reaches 7.5～9.0, and the response time keeps more than 5～10 minutes；
(4) heat temperature raising, makes methanol distill out, and methanol is carried out with cooling recovery；
(5) when temperature reaches 75～85 DEG C, then recovered under reduced pressure, when vacuum is not less than 0.08mpa, 125 DEG C～135 DEG C of temperature
When, stop heating, continue vacuum 60～120 minutes, final temperature keeps 125 DEG C～140 DEG C, regard in cylinder no distillation as
Only, release vacuum, cooling had both obtained hexamethylol melamine resin.
Claims (1)
1. the preparation method of rubber adhesive hmmm is it is characterised in that comprise the following steps:
(1) water, paraformaldehyde are added in a kettle., it is 7～8 that hydro-oxidation sodium adjusts ph value, after stirring, then puts into melamine
Amine, is heated to 40～50 DEG C, is incubated 30 minutes～100 minutes；Adjusting ph value with sodium hydroxide is 8～10, is then heated to 50
～80 DEG C, it is incubated 30 minutes～100 minutes；It is down to 40 DEG C；Adjust ph with sulphuric acid to neutrality；
(2) add methanol in a kettle., under stirring；Reactor begins to warm up, and when temperature reaches 48～58 DEG C, adds sulfur
Acid carries out etherification reaction, and 2～3, temperature keeps constant to ph, after material becomes clear, continues insulation 60～120 minutes；
(3) keeping temperature, adds sodium hydroxide neutralization, and ph reaches 7.5～9.0, and the response time keeps more than 5～10 minutes；
(4) heat temperature raising, makes methanol distill out, and methanol is carried out with cooling recovery；
(5) when temperature reaches 75～85 DEG C, then recovered under reduced pressure, when vacuum is not less than 0.08mpa, 125 DEG C～135 DEG C of temperature
When, stop heating, continue vacuum 60～120 minutes, final temperature keeps 125 DEG C～140 DEG C, regard in cylinder no distillation as
Only, release vacuum, cooling had both obtained hexamethylol melamine resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610714987.2A CN106349444A (en) | 2016-08-25 | 2016-08-25 | Preparation method of rubber adhesive HMMM (Hexamethoxy Methyl Melamine) |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610714987.2A CN106349444A (en) | 2016-08-25 | 2016-08-25 | Preparation method of rubber adhesive HMMM (Hexamethoxy Methyl Melamine) |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106349444A true CN106349444A (en) | 2017-01-25 |
Family
ID=57844013
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610714987.2A Pending CN106349444A (en) | 2016-08-25 | 2016-08-25 | Preparation method of rubber adhesive HMMM (Hexamethoxy Methyl Melamine) |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106349444A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108624269A (en) * | 2018-04-20 | 2018-10-09 | 兰溪市克莱森助剂有限公司 | A kind of rubber adhesive and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101333198A (en) * | 2008-07-02 | 2008-12-31 | 张家港顺昌化工有限公司 | Method for preparing HMMM resin |
| CN101619126A (en) * | 2009-07-31 | 2010-01-06 | 常州曙光化工厂 | Method for preparing melamine formaldehyde resin for rubber |
| CN101696258A (en) * | 2009-10-11 | 2010-04-21 | 江苏国立化工科技有限公司 | Method for improving etherification degree of hexa-methoxy methyl melamine resin |
| CN101786995A (en) * | 2010-03-11 | 2010-07-28 | 浙江奥仕化学有限公司 | Method for preparing granular hexamethylol melamine |
| CN103086992A (en) * | 2012-11-14 | 2013-05-08 | 江苏国立化工科技有限公司 | Preparation method of hexamethoxymethyl melamine resin |
-
2016
- 2016-08-25 CN CN201610714987.2A patent/CN106349444A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101333198A (en) * | 2008-07-02 | 2008-12-31 | 张家港顺昌化工有限公司 | Method for preparing HMMM resin |
| CN101619126A (en) * | 2009-07-31 | 2010-01-06 | 常州曙光化工厂 | Method for preparing melamine formaldehyde resin for rubber |
| CN101696258A (en) * | 2009-10-11 | 2010-04-21 | 江苏国立化工科技有限公司 | Method for improving etherification degree of hexa-methoxy methyl melamine resin |
| CN101786995A (en) * | 2010-03-11 | 2010-07-28 | 浙江奥仕化学有限公司 | Method for preparing granular hexamethylol melamine |
| CN103086992A (en) * | 2012-11-14 | 2013-05-08 | 江苏国立化工科技有限公司 | Preparation method of hexamethoxymethyl melamine resin |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108624269A (en) * | 2018-04-20 | 2018-10-09 | 兰溪市克莱森助剂有限公司 | A kind of rubber adhesive and preparation method thereof |
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| C06 | Publication | ||
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170125 |
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