CN102432821A - Novel preparation method of environment-friendly type MDI (4,4-Diphenylmethane Diisocyanate)-TMP (Trimethoprim) curing agent - Google Patents
Novel preparation method of environment-friendly type MDI (4,4-Diphenylmethane Diisocyanate)-TMP (Trimethoprim) curing agent Download PDFInfo
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- CN102432821A CN102432821A CN2011102460186A CN201110246018A CN102432821A CN 102432821 A CN102432821 A CN 102432821A CN 2011102460186 A CN2011102460186 A CN 2011102460186A CN 201110246018 A CN201110246018 A CN 201110246018A CN 102432821 A CN102432821 A CN 102432821A
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Abstract
The invention discloses a novel preparation method of an environment-friendly type MDI (4,4-Diphenylmethane Diisocyanate)-TMP (Trimethoprim) curing agent. The novel preparation method comprises the following steps of: a, preparing an MDI soiution: adding ethyl acetate into a reaction kettle filled with nitrogen gas or carbon dioxide, then adding MDI and a small amount of catalyst, raising the temperature to be 50-60DEG C, simultaneously stirring to be completely dissolved and preserving the heat for 1-2 hours; b, preparing a TMP soiution: adding ethyl acetate or TMP into another vessel, raising the temperature to be 40-50DEG C and stirring to be completely dissolved to obtain the TMP solution; and c,. adding the TMP solution in the MDI solution in the step a, carrying out a heat preserving reaction at 70DEG C for 1-5 hours and then adding a small amount of polymerization inhibitor. The environment-friendly type MDI-TMP curing agent obtained in the invention has the advantages of fewer side reactions, relatively-high content of -NCO, white color and wider application range.
Description
Technical field
The invention belongs to chemical field, relate in particular to the compound 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 have 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, and the MDI-TMP solidifying agent that common working method obtains is light yellow transparent liquid or yellow transparent liquid, and this is because of oxidized causing in the reaction process.When some purposes required water white transparency, this MDI-TMP solidifying agent just can't be suitable for.
Summary of the invention
Goal of the invention: the defective to above-mentioned existence the invention provides a kind of method for preparing water white MDI and TMP solidifying agent.
Technical scheme: for realizing the foregoing invention purpose; The present invention adopts following technical scheme: a kind of new preparation process of environment-friendly type MDI-TMP solidifying agent; May further comprise the steps: the preparation of a, MDI solution: in reaction kettle, add vinyl acetic monomer, add 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 other container, add vinyl acetic monomer or, add TMP again, 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 following insulation reaction 1 ~ 5 hour, add a spot of stopper then, be full of nitrogen or carbonic acid gas in the said reaction kettle.
Said catalyzer is Lithium Oxide 98min, epoxyeicosatrienoic acid zinc or dodecyl dimethyl tertiary amine.
Said stopper is phosphoric acid, oxalic acid or Hydrocerol A.
Beneficial effect: compared with prior art; The present invention has the following advantages: when TMP and MDI building-up reactions, be full of nitrogen or carbonic acid gas in the reaction kettle, can prevent that airborne oxygen is with the product oxidation; Thereby obtain water white MDI-TMP solidifying agent, can be suitable for purposes widely.
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 being full of the reaction kettle of nitrogen, adds 15 parts adds 30 parts MDI and little amount of catalyst again, and is full of nitrogen, is warming up to 50 ~ 60 ℃, is stirred to dissolving fully simultaneously, and is incubated 1 ~ 2h acquisition 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 the water white transparent liquid under the normal temperature, and solid content is 73%, and viscosity is 1400 ~ 1500mPa.s, and-NCO content is 11.0 ~ 11.5%, and the free TDI monomer content is less than 0.05%.The MDI-TMP solidifying agent that obtains does not all occur solidifying through depositing 1 year, and viscosity is about 1500 mPa.s.
Claims (3)
1. the new preparation process of environment-friendly type MDI-TMP solidifying agent may further comprise the steps: the preparation of a, MDI solution: in reaction kettle, add vinyl acetic monomer, add 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 other container, add vinyl acetic monomer or, add TMP again, 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 following insulation reaction 1 ~ 5 hour, add a spot of stopper then, it is characterized in that: be full of nitrogen or carbonic acid gas in the said reaction kettle.
2. the new preparation process of environment-friendly type MDI-TMP solidifying agent according to claim 1 is characterized in that: said catalyzer is Lithium Oxide 98min, epoxyeicosatrienoic acid zinc or dodecyl dimethyl tertiary amine.
3. the new preparation process of environment-friendly type MDI-TMP solidifying agent according to claim 1 is characterized in that: said stopper is phosphoric acid, oxalic acid or Hydrocerol A.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102460186A CN102432821A (en) | 2011-08-25 | 2011-08-25 | Novel preparation method of environment-friendly type MDI (4,4-Diphenylmethane Diisocyanate)-TMP (Trimethoprim) curing agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102460186A CN102432821A (en) | 2011-08-25 | 2011-08-25 | Novel preparation method of environment-friendly type MDI (4,4-Diphenylmethane Diisocyanate)-TMP (Trimethoprim) curing agent |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102432821A true CN102432821A (en) | 2012-05-02 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011102460186A Pending CN102432821A (en) | 2011-08-25 | 2011-08-25 | Novel preparation method of environment-friendly type MDI (4,4-Diphenylmethane Diisocyanate)-TMP (Trimethoprim) curing agent |
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| CN (1) | CN102432821A (en) |
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 (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1357558A (en) * | 2000-12-05 | 2002-07-10 | 上海市涂料研究所 | Paint curing agent 4,4'-diphenyl methane diisocyanate prepolymer and its prepn |
| CN101230124A (en) * | 2007-01-27 | 2008-07-30 | 周建明 | Curing agent 4,4'-biphenyl methane diisocyanate prepolymer and preparation method thereof |
-
2011
- 2011-08-25 CN CN2011102460186A patent/CN102432821A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1357558A (en) * | 2000-12-05 | 2002-07-10 | 上海市涂料研究所 | Paint curing agent 4,4'-diphenyl methane diisocyanate prepolymer and its prepn |
| CN101230124A (en) * | 2007-01-27 | 2008-07-30 | 周建明 | Curing agent 4,4'-biphenyl methane diisocyanate prepolymer and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 周俊锋等: "环保型双组分聚氨酯固化剂MDI/TMP的开发及应用", 《涂料工业》 * |
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: 20120502 |