CN102352019A - Environment-friendly MDI-TMP polymerization inhibitor - Google Patents
Environment-friendly MDI-TMP polymerization inhibitor Download PDFInfo
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- CN102352019A CN102352019A CN2011102517216A CN201110251721A CN102352019A CN 102352019 A CN102352019 A CN 102352019A CN 2011102517216 A CN2011102517216 A CN 2011102517216A CN 201110251721 A CN201110251721 A CN 201110251721A CN 102352019 A CN102352019 A CN 102352019A
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Abstract
The invention discloses an environment-friendly MDI-TMP polymerization inhibitor. The polymerization inhibitor is prepared through steps that: a, part of a reaction solvent is added into a reaction vessel; MDI and a catalyst are added into the reaction vessel; the temperature in the reaction vessel is increased to 50 to 60 DEG C; the materials are stirred until completely dissolved; and the temperature of the solution is maintained for 1 to 2 hours; b, TMP is added to rest of the reaction solvent; the temperature is increased to 40 to 50 DEG C, and the materials are completely dissolved by stirring, such that a TMP solution is obtained; c, the TMP solution obtained in the step a is added to the MDI solution, and the temperature of the mixture is maintained for 1 to 5 hours; a polymerization inhibitor is added to the mixture; and the obtained product is cooled and packaged. The MDI-TMP polymerization inhibitor is prepared from materials of, by weight: 20 to 540 parts of MDI, 10 to 20 parts of TMP, 10 to 30 parts of a reaction solvent, and trace of a catalyst and a polymerization inhibitor. The content of toxic free TDI in the MDI-TMP polymerization inhibitor provided by the invention is low. Therefore, the MDI-TMP polymerization inhibitor is environment-friendly, and has long storage life.
Description
Technical field
The invention belongs to chemical field, relate in particular to coating and synthesize.
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, therefore how reducing free TDI content is a present trend with the TDI-TMP solidifying agent that obtains environment-friendly type.The solidifying agent of in use hoping environment-friendly type in addition has high stability, and preservation period is enough long.
Summary of the invention
Goal of the invention: the present invention is directed to the deficiency of prior art, a kind of low-free TDI content is provided, the environment-friendly type MDI-TMP stopper that the shelf lives is long.
Technical scheme: for realizing the foregoing invention purpose, the present invention adopts following technical scheme: a kind of environment-friendly type MDI-TMP stopper is characterized in that: said MDI-TMP stopper is indefinite composition, and this MDI-TMP bridging agent is prepared by following method:
A. the preparation of MDI solution: in reaction kettle, add the partial reaction solvent, add MDI and catalyzer again, be warming up to 50 ~ 60 ℃, be stirred to dissolving fully simultaneously, and be incubated 1 ~ 2h;
B. the preparation of TMP solution: in the residue reaction solvent, add 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, be incubated 1 ~ 5 hour down at 60 ~ 80 ℃;
D. in the solution that step c obtains, add stopper, cooling back packing; Wherein, among the preparation method of above-mentioned MDI-TMP bridging agent, the addition of each material by weight: MDI is 20 ~ 50 parts, and TMP is 10 ~ 20 parts, and reaction solvent is 10 ~ 30 parts, the addition of catalyzer and stopper be the trace.
Reaction solvent among the said preparation method is ethyl acetate, vinyl acetic monomer or alcohols.
Stopper among the said preparation method is phosphoric acid, oxalic acid or Hydrocerol A.
As preferably, among the preparation method of said MDI-TMP bridging agent, the addition of each material by weight: MDI is 30 parts, and TMP is 15 parts, and reaction solvent is 20 parts, the addition of catalyzer and stopper.
Beneficial effect: compared with prior art, the present invention has the following advantages: the free TDI content in the MDI-TMP type solidifying agent that the present invention obtains is far below TDI-TMP type bridging agent; Can prevent that through adding stopper the MDI-TMP stopper takes place to solidify by phenomenon, the shelf lives of improving MDI-TMP in the deposit process.
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
After dropping into 5 parts of the vinyl acetic monomers of organic solvent technical grade in the earlier clean container, adds 15 parts technical grade TMP, elevated temperature to 40 ℃ is opened stirring simultaneously and dissolved fully up to TMP and obtain TMP solution, and is for use; In reaction kettle, add 15 parts of the vinyl acetic monomers of organic solvent technical grade in addition, and add 30 parts MDI and appropriate amount of catalysts Lithium Oxide 98min, elevated temperature to 40 ℃ stirs fully simultaneously and dissolves, and promptly gets MDI solution; In above-mentioned MDI solution, add TMP solution then, this moment elevated temperature to 70 ℃, reaction 2h adds a spot of phosphoric acid at last, stirs and promptly gets the MDI-TMP stopper.
Through detecting, the technical indicator of gained MDI-TMP stopper is following: outward appearance is yellow transparent liquid under the normal temperature, and solid content is 72%, and viscosity is 1300 ~ 1400mPa.s, and the free TDI monomer content is 0.054%.The MDI-TMP stopper that obtains does not all occur solidifying through depositing 1 year, and viscosity is about 14000 mPa.s.
Embodiment 2 ~ 4
The production craft step of embodiment 2 ~ 4 is identical with embodiment 1, has only each material input amount different with reaction parameter, particular case such as table 1 and table 2.
Each material input amount among table 1: the embodiment 2 ~ 4.
Reaction parameter among table 2: the embodiment 2 ~ 4.
The technical indicator such as the table 3 of the MDI-TMP stopper that obtains through aforesaid method.
| ? | Outward appearance | Solid content | Viscosity | The free TDI monomer content | Storage time |
| Embodiment 2 | Light yellow transparent liquid | 72% | 1450mPa.·s | 0.055 | 1 year uncured |
| Embodiment 3 | Yellow transparent liquid | 74% | 1500mPa.·s | 0.045 | 1 year uncured |
| Embodiment 4 | Yellow transparent liquid | 73% | 1700mPa.·s | 0.024 | 1 year uncured |
The technical indicator of the MDI-TMP stopper that table 3: embodiment 2 ~ 4 obtains.
Claims (4)
1. environment-friendly type MDI-TMP stopper, it is characterized in that: said MDI-TMP stopper is indefinite composition, this MDI-TMP bridging agent is prepared by following method:
A. the preparation of MDI solution: in reaction kettle, add the partial reaction solvent, add MDI and catalyzer again, be warming up to 50 ~ 60 ℃, be stirred to dissolving fully simultaneously, and be incubated 1 ~ 2h;
B. the preparation of TMP solution: in the residue reaction solvent, add 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, be incubated 1 ~ 5 hour down at 60 ~ 80 ℃;
D. in the solution that step c obtains, add stopper, cooling back packing;
Wherein, among the preparation method of above-mentioned MDI-TMP bridging agent, the addition of each material by weight: MDI is 20 ~ 50 parts, and TMP is 10 ~ 20 parts, and reaction solvent is 10 ~ 30 parts, the addition of catalyzer and stopper be the trace.
2. environment-friendly type MDI-TMP stopper according to claim 1 is characterized in that: the reaction solvent among the said preparation method is ethyl acetate, vinyl acetic monomer or alcohols.
3. environment-friendly type MDI-TMP stopper according to claim 1 is characterized in that: the stopper among the said preparation method is phosphoric acid, oxalic acid or Hydrocerol A.
4. environment-friendly type MDI-TMP stopper according to claim 1; It is characterized in that: among the preparation method of said MDI-TMP bridging agent, the addition of each material by weight: MDI is 30 parts, and TMP is 15 parts; Reaction solvent is 20 parts, and catalyzer and stopper are on a small quantity.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102517216A CN102352019A (en) | 2011-08-30 | 2011-08-30 | Environment-friendly MDI-TMP polymerization inhibitor |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102517216A CN102352019A (en) | 2011-08-30 | 2011-08-30 | Environment-friendly MDI-TMP polymerization inhibitor |
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| CN102352019A true CN102352019A (en) | 2012-02-15 |
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| CN2011102517216A Pending CN102352019A (en) | 2011-08-30 | 2011-08-30 | Environment-friendly MDI-TMP polymerization inhibitor |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101230124A (en) * | 2007-01-27 | 2008-07-30 | 周建明 | Curing agent 4,4'-biphenyl methane diisocyanate prepolymer and preparation method thereof |
| CN102352017A (en) * | 2011-08-25 | 2012-02-15 | 吴江市北厍盛源纺织品助剂厂 | Method for preparing environmentally-friendly diphenyl methane diisocyanate-trimethoprim (MDI-TMP) curing agent |
| CN102352015A (en) * | 2011-08-25 | 2012-02-15 | 吴江市北厍盛源纺织品助剂厂 | Improved method for preparing environment-friendly diphenylmethane diisocyanate-trimethylolpropane (MDI-TMP) curing agent |
| CN102432821A (en) * | 2011-08-25 | 2012-05-02 | 吴江市北厍盛源纺织品助剂厂 | Novel preparation method of environment-friendly type MDI (4,4-Diphenylmethane Diisocyanate)-TMP (Trimethoprim) curing agent |
-
2011
- 2011-08-30 CN CN2011102517216A patent/CN102352019A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101230124A (en) * | 2007-01-27 | 2008-07-30 | 周建明 | Curing agent 4,4'-biphenyl methane diisocyanate prepolymer and preparation method thereof |
| CN102352017A (en) * | 2011-08-25 | 2012-02-15 | 吴江市北厍盛源纺织品助剂厂 | Method for preparing environmentally-friendly diphenyl methane diisocyanate-trimethoprim (MDI-TMP) curing agent |
| CN102352015A (en) * | 2011-08-25 | 2012-02-15 | 吴江市北厍盛源纺织品助剂厂 | Improved method for preparing environment-friendly diphenylmethane diisocyanate-trimethylolpropane (MDI-TMP) curing agent |
| CN102432821A (en) * | 2011-08-25 | 2012-05-02 | 吴江市北厍盛源纺织品助剂厂 | Novel preparation method of environment-friendly type MDI (4,4-Diphenylmethane Diisocyanate)-TMP (Trimethoprim) curing agent |
Non-Patent Citations (1)
| Title |
|---|
| 周峻峰 等，: "环保型双组分聚氨酯固化剂MDI/TMP的开发及应用", 《涂料工业》, vol. 40, no. 7, 31 July 2010 (2010-07-31) * |
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Application publication date: 20120215 |