CN102352017A - Method for preparing environmentally-friendly diphenyl methane diisocyanate-trimethoprim (MDI-TMP) curing agent - Google Patents
Method for preparing environmentally-friendly diphenyl methane diisocyanate-trimethoprim (MDI-TMP) curing agent Download PDFInfo
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- CN102352017A CN102352017A CN2011102460218A CN201110246021A CN102352017A CN 102352017 A CN102352017 A CN 102352017A CN 2011102460218 A CN2011102460218 A CN 2011102460218A CN 201110246021 A CN201110246021 A CN 201110246021A CN 102352017 A CN102352017 A CN 102352017A
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Abstract
The invention discloses a method for preparing an environmentally-friendly diphenyl methane diisocyanate-trimethoprim (MDI-TMP) curing agent. The method comprises the following steps of: a, preparing MDI solution, adding 15 parts of acetic ether into a reaction kettle, adding 30 parts of MDI and a little amount of catalyst, heating the solution to the temperature of between 50 and 60 DEG C, stirring till full dissolving, and performing heat preservation for 1 to 2 hours; b, preparing TMP solution, adding 10 parts of TMP into 10 parts of acetic ether, heating the solution to the temperature of between 40 and 50 DEG C, stirring till full dissolving, and obtaining the TMP solution; and c, slowly dripping the TMP solution into the MDI solution for 1 to 2 hours, performing heat preservation reaction for 4 hours at the temperature of 70 DEG C, and adding a little amount of polymerization inhibitor, wherein the TMP solution is gradually added in the step c of the preparation method. The obtained MDI-TMP curing agent has little side reaction and relatively high -NCO content.
Description
Technical field
The invention belongs to chemical field, relate in particular to the synthesis method of MDI-TMP solidifying agent.
Background technology
Polyurethane coating is one type of excellent property, widely used coating.Because therefore its paint film good mechanical property, tough and tensile, wear-resisting, plentiful, bright can have the wide application of sending out in the field at coatings decoration, synthon in low-temperature curing.Solidifying agent is the important component part in the double-component polyurethane coating; And TDI-TMP type solidifying agent is wherein most widely used a kind of; But because the TDI monomer of TDI-TMP solidifying agent is a kind of noxious chemical; In use inevitably there is free TDI; Very big to human harm; The free TDI content of the TDI-TMP type bridging agent of domestic production at present is many 2 ~ 5%; Along with the enhancing of environmental protection consciousness, how reducing free TDI content is a present trend with the TDI-TMP solidifying agent that obtains environment-friendly type.And the solidifying agent of MDI-TMP type is because its hypotoxicity; More and more paid close attention to; Especially the preparation method is updating always; TMP injected volume is big among the present preparation method; It is local excessive to cause easily, the large percentage of side reaction, in the MDI-TMP solidifying agent of acquisition-NCO content generally has only 9.0 ~ 10.5%; And-NCO content is high more, and its subsequent product generally can be good more.
Summary of the invention
Goal of the invention:, the invention provides a kind of efficient MDI and TMP building-up reactions of low side reaction to the defective of above-mentioned existence.
Technical scheme: for realizing the foregoing invention purpose; The present invention adopts following technical scheme: a kind of preparation environment-friendly type MDI-TMP solidifying agent method; May further comprise the steps: the preparation of a, MDI solution: the vinyl acetic monomer that in reaction kettle, adds 15 parts; The MDI and the little amount of catalyst that add 30 parts again; Be warming up to 50 ~ 60 ℃; Be stirred to dissolving fully simultaneously, and be incubated 1 ~ 2h; The preparation of b, TMP solution: in 10 parts vinyl acetic monomer, add 10 parts of TMP, be warming up to 40 ~ 50 ℃, being stirred to fully, dissolving obtains TMP solution; C, in MDI solution, add TMP solution described in the step a, 70 ℃ of insulations 4 hours down, add a spot of stopper then, it is characterized in that: the interpolation of TMP solution is progressively to add among said preparing method's step c.
The adding of TMP is adopted slowly and is dripped among the said step c, and this dropping process time is 1 ~ 2 hour.
Beneficial effect: compared with prior art; The present invention has the following advantages: TMP solution is taked slowly to add to make heat of reaction can have time enough to dissipate; Never can cause excessive temperature to raise, cause the generation of side reaction, simultaneously in the product of Huo Deing-NCO is higher relatively.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is elaborated, but protection scope of the present invention is not limited to said embodiment.
Embodiment 1
The vinyl acetic monomer that in reaction kettle, adds 15 parts adds 30 parts MDI and little amount of catalyst again, is warming up to 50 ~ 60 ℃, is stirred to dissolving fully simultaneously, and is incubated 1 ~ 2h and obtains MDI solution; Add 10 parts of TMP in 10 parts the vinyl acetic monomer, be warming up to 40 ~ 50 ℃, being stirred to fully, dissolving obtains TMP solution; In MDI solution, slowly drip TMP solution then, the time of this dropping process is 1 ~ ~ 2 hour, 70 ℃ of following insulation reaction 4 hours, adds a spot of stopper then at last.
Through detecting, the technical indicator of gained MDI-TMP solidifying agent is following: outward appearance is light yellow transparent liquid under the normal temperature, and solid content is 72%, and viscosity is 1450mPa.s, and-NCO content is 11.5 ~ 12.8%, and the free TDI monomer content is 0.054%.The MDI-TMP solidifying agent that obtains does not all occur solidifying through depositing 1 year, and viscosity is about 1400 mPa.s.
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Claims (2)
1. one kind prepares environment-friendly type MDI-TMP solidifying agent method; May further comprise the steps: the preparation of a, MDI solution: in reaction kettle, add 15 parts vinyl acetic monomer, add 30 parts MDI and little amount of catalyst again, be warming up to 50 ~ 60 ℃; Be stirred to dissolving fully simultaneously, and be incubated 1 ~ 2h; The preparation of b, TMP solution: in 10 parts vinyl acetic monomer, add 10 parts of TMP, be warming up to 40 ~ 50 ℃, being stirred to fully, dissolving obtains TMP solution; C, in MDI solution, add TMP solution described in the step a, 70 ℃ of insulations 4 hours down, add a spot of stopper then, it is characterized in that: the interpolation of TMP solution is progressively to add among said preparing method's step c.
2. preparation environment-friendly type MDI-TMP solidifying agent method according to claim 1 is characterized in that: the adding of TMP is adopted slowly and is dripped among the said step c, and this dropping process time is 1 ~ 2 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102460218A CN102352017A (en) | 2011-08-25 | 2011-08-25 | Method for preparing environmentally-friendly diphenyl methane diisocyanate-trimethoprim (MDI-TMP) curing agent |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102460218A CN102352017A (en) | 2011-08-25 | 2011-08-25 | Method for preparing environmentally-friendly diphenyl methane diisocyanate-trimethoprim (MDI-TMP) curing agent |
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| CN102352017A true CN102352017A (en) | 2012-02-15 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2011102460218A Pending CN102352017A (en) | 2011-08-25 | 2011-08-25 | Method for preparing environmentally-friendly diphenyl methane diisocyanate-trimethoprim (MDI-TMP) curing agent |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102352019A (en) * | 2011-08-30 | 2012-02-15 | 吴江市北厍盛源纺织品助剂厂 | Environment-friendly MDI-TMP polymerization inhibitor |
| CN103145947A (en) * | 2013-02-25 | 2013-06-12 | 晋江市华福化工有限公司 | Novel environmental-friendly curing agent and preparation method for same |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060241199A1 (en) * | 2004-10-15 | 2006-10-26 | Danisco A/S | Foamed isocyanate-based polymer, a mix and process for production thereof |
| CN101230124A (en) * | 2007-01-27 | 2008-07-30 | 周建明 | Curing agent 4,4'-biphenyl methane diisocyanate prepolymer and preparation method thereof |
| CN101307127A (en) * | 2008-07-16 | 2008-11-19 | 武汉仕全兴装饰涂料有限公司 | Polyurethane curing agent with low free MDI monomer and method for preparing same |
-
2011
- 2011-08-25 CN CN2011102460218A patent/CN102352017A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060241199A1 (en) * | 2004-10-15 | 2006-10-26 | Danisco A/S | Foamed isocyanate-based polymer, a mix and process for production thereof |
| CN101230124A (en) * | 2007-01-27 | 2008-07-30 | 周建明 | Curing agent 4,4'-biphenyl methane diisocyanate prepolymer and preparation method thereof |
| CN101307127A (en) * | 2008-07-16 | 2008-11-19 | 武汉仕全兴装饰涂料有限公司 | Polyurethane curing agent with low free MDI monomer and method for preparing same |
Non-Patent Citations (1)
| Title |
|---|
| 《涂料工业》 20100731 周俊锋 等 环保型双组分聚氨酯固化剂MDI/TMP的开发及应用 1-2 第40卷, 第7期 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102352019A (en) * | 2011-08-30 | 2012-02-15 | 吴江市北厍盛源纺织品助剂厂 | Environment-friendly MDI-TMP polymerization inhibitor |
| CN103145947A (en) * | 2013-02-25 | 2013-06-12 | 晋江市华福化工有限公司 | Novel environmental-friendly curing agent and preparation method for same |
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Application publication date: 20120215 |