CN102417581A - Preparation method for organic silicon modified polyurethane (PU) finishing agent - Google Patents
Preparation method for organic silicon modified polyurethane (PU) finishing agent Download PDFInfo
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- CN102417581A CN102417581A CN2011103380668A CN201110338066A CN102417581A CN 102417581 A CN102417581 A CN 102417581A CN 2011103380668 A CN2011103380668 A CN 2011103380668A CN 201110338066 A CN201110338066 A CN 201110338066A CN 102417581 A CN102417581 A CN 102417581A
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Abstract
The invention discloses organic silicon modified polyurethane (PU) finishing agent and a preparation method thereof. The preparation method comprises the following steps: adding N- methyl pyrrolidone, 4,4'-diphenylmethane diisocyanate (MDI) and dibutyltin dilaurate of the catalytic amount in a reaction kettle filled with inert gas; heating and dissolving under the condition of stirring; slowly adding trimethylolpropane (TMP) and 1,4- butanediol; reacting for 1-5h at the temperature of 60-90DEG C to obtain a pre-polymerization product; then, adding mono-hydroxy polyethylene oxide and 1,3- dihydroxyl trimethylacetic acid; keeping temperature to react for 1-2h to obtain terminated polyurethane; then , continuously adding ethidene diamine chain extender; finally, adding 3-amino propyl triethoxy silane KH-550 to carry out polymerization reaction for 1-3h; and continuously adding a proper quantity of stabilizing agent to obtain a modified polyurethane product. The organic silicon modified PU finishing agent obtained by the invention has the advantages of low free toluene diisocynate (TDI), smooth leather glaze, and soft, plump and elastic leather bodies, and the water resistance, the oil-proof performance and the abrasion performance of the leather can be improved.
Description
Technical field:
The present invention relates to a kind of organic-silicon-modified polyurethane PU finish, the preparation method of particularly organic-silicon-modified polyurethane PU finish.
Background technology:
Polyaminoester emulsion has advantages such as light, Bearable dry and wet wipe as film forming material, the whitewashing that is widely used in various clothing leathers, upper leather, luggage leather, glove leather automotive seat leather etc. is used, and polyaminoester emulsion is usually with monomer 2; 4 '-tolylene diisocyanate (TDI), polyethers (polyester) polyvalent alcohol is the pre-polymerization main raw material, because the toxicity of TDI is high; Environment is caused very big harm; And, cover with paint, lacquer, colour wash, etc. in the technology at PU, be prone to cause leather finish top layer feel and water-repellancy undesirable.
This experiment is first with 4,4 '-'-diphenylmethane diisocyanate (MDI), and TMP, 1, the 4-butyleneglycol, the monohydroxy polyethylene oxide, 1, the prepolymerization of 3-dihydroxyl trimethylacetic acid is introduced organosilicon again the polyurethane polyureas zoarium is carried out modification.
Summary of the invention:
Goal of the invention: the defective to prior art exists the invention provides a kind of organic-silicon-modified polyurethane PU finish and preparation method thereof.
Technical scheme: for realizing the foregoing invention purpose; The present invention adopts following technical scheme: a kind of organic-silicon-modified polyurethane PU finish and preparation method thereof; May further comprise the steps: in being full of the reaction kettle of rare gas element, add the dibutyl tin laurate of organic solvent N-Methyl pyrrolidone, MDI and catalytic amount, stir heating for dissolving down; Slowly add TMP and 1 then, the 4-butyleneglycol obtains prepolymer product at 60 ~ 90 ℃ of reaction 1 ~ 5h; Then add end-capping reagent monohydroxy polyethylene oxide and 1,3-dihydroxyl trimethylacetic acid, insulation reaction 1 ~ 2h obtains end capped urethane; Continue to add the quadrol chainextender; Add 3-aminopropyltriethoxywerene werene KH-550 at last, polyreaction 1 ~ 3h continues to add an amount of stablizer, gets the modified polyurethane product.
The mol ratio of said MDI and TMP is 1 ~ 2:1.
Said end-capping reagent monohydroxy polyethylene oxide and 1, the mass ratio of 3-dihydroxyl trimethylacetic acid is 10 ~ 40:1.
The mass ratio of said 3-aminopropyltriethoxywerene werene and blocked polyurethane is 1:10 ~ 30.
Beneficial effect: compared with prior art, the present invention has the following advantages: the present invention obtains organic-silicon-modified polyurethane PU finish and has low-free TDI, safety and environmental protection; Leather light face is smooth; The leather body is soft, and is plentiful and the leather silk-like handle is given in high resilience; Improve the water-repellancy of leather, grease proofness and wear resisting property.
Embodiment:
Below in conjunction with embodiment the present invention is done detailed description further, but the scope that the present invention requires to protect is not limited to the scope that embodiment representes.
Embodiment 1:
Adding organic solvent N-Methyl pyrrolidone (85kg) and MDI in the reaction kettle that is full of nitrogen or rare gas element (1.0kmol, 254kg), the dibutyl tin laurate of catalytic amount (1.5kg) is heated to 70 ℃ of dissolvings under stirring; In reaction kettle, drip TMP (1.05kmol), 1,4-butyleneglycol (0.25kmol), controlled temperature drip and finish at 70 ~ 95 ℃; Insulation reaction 1 ~ 5h adds end-capping reagent monohydroxy polyethylene oxide (280kg) and 1 at 90 ~ 135 ℃, 3-dihydroxyl trimethylacetic acid (20kg), reaction 1 ~ 2h; Be cooled to 80 ℃, add neutralizing agent quadrol (8.5kg), J adds KH-550, reaction 2h; Add stablizer (0.5kg), high-speed stirring is reduced to 20 ℃, encapsulating products.
Claims (4)
1. organic-silicon-modified polyurethane PU finish and preparation method thereof may further comprise the steps: in being full of the reaction kettle of rare gas element, add the dibutyl tin laurate of organic solvent N-Methyl pyrrolidone, MDI and catalytic amount, stir heating for dissolving down; Slowly add TMP and 1 then, the 4-butyleneglycol obtains prepolymer product at 60 ~ 90 ℃ of reaction 1 ~ 5h; Then add end-capping reagent monohydroxy polyethylene oxide and 1,3-dihydroxyl trimethylacetic acid, insulation reaction 1 ~ 2h obtains end capped urethane; Continue to add the quadrol chainextender; Add 3-aminopropyltriethoxywerene werene KH-550 at last, polyreaction 1 ~ 3h continues to add an amount of stablizer, gets the modified polyurethane product.
2. according to the said a kind of organic-silicon-modified polyurethane PU finish preparation method of claim 1, it is characterized in that: the mol ratio of said MDI and TMP is 1 ~ 2:1.
3. according to the said a kind of organic-silicon-modified polyurethane PU finish preparation method of claim 1, it is characterized in that: said end-capping reagent monohydroxy polyethylene oxide and 1, the mass ratio of 3-dihydroxyl trimethylacetic acid is 10 ~ 40:1.
4. according to the said a kind of organic-silicon-modified polyurethane PU finish preparation method of claim 1, it is characterized in that: the mass ratio of said 3-aminopropyltriethoxywerene werene and blocked polyurethane is 1:10 ~ 30.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103380668A CN102417581A (en) | 2011-11-01 | 2011-11-01 | Preparation method for organic silicon modified polyurethane (PU) finishing agent |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103380668A CN102417581A (en) | 2011-11-01 | 2011-11-01 | Preparation method for organic silicon modified polyurethane (PU) finishing agent |
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| CN102417581A true CN102417581A (en) | 2012-04-18 |
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| CN2011103380668A Pending CN102417581A (en) | 2011-11-01 | 2011-11-01 | Preparation method for organic silicon modified polyurethane (PU) finishing agent |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102898934A (en) * | 2012-09-11 | 2013-01-30 | 青岛文创科技有限公司 | Polyurethane sealing and repairing agent |
| CN103755914A (en) * | 2013-12-20 | 2014-04-30 | 苏州市万泰真空炉研究所有限公司 | Preparation method of light-stable polyurethane hard foamed plastic |
| CN106928421A (en) * | 2017-04-13 | 2017-07-07 | 合肥科天水性科技有限责任公司 | A kind of clothing leather soft bed material and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1854165A (en) * | 2005-04-20 | 2006-11-01 | 广州宏昌胶粘带厂 | Organic silicon modified aqueous polyurethane |
| CN101845269A (en) * | 2010-05-31 | 2010-09-29 | 淄博永麒化工技术开发有限公司 | Waterborne polyurethane finishing agent for PVC (Polyvinyl Chloride) protective gloves and preparation method thereof |
| CN102093538A (en) * | 2010-12-16 | 2011-06-15 | 温州市登达化工有限公司 | Synthesis process of organosilicon-modified single-component aqueous polyurethane coating agent |
-
2011
- 2011-11-01 CN CN2011103380668A patent/CN102417581A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1854165A (en) * | 2005-04-20 | 2006-11-01 | 广州宏昌胶粘带厂 | Organic silicon modified aqueous polyurethane |
| CN101845269A (en) * | 2010-05-31 | 2010-09-29 | 淄博永麒化工技术开发有限公司 | Waterborne polyurethane finishing agent for PVC (Polyvinyl Chloride) protective gloves and preparation method thereof |
| CN102093538A (en) * | 2010-12-16 | 2011-06-15 | 温州市登达化工有限公司 | Synthesis process of organosilicon-modified single-component aqueous polyurethane coating agent |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102898934A (en) * | 2012-09-11 | 2013-01-30 | 青岛文创科技有限公司 | Polyurethane sealing and repairing agent |
| CN103755914A (en) * | 2013-12-20 | 2014-04-30 | 苏州市万泰真空炉研究所有限公司 | Preparation method of light-stable polyurethane hard foamed plastic |
| CN103755914B (en) * | 2013-12-20 | 2016-11-16 | 苏州市万泰真空炉研究所有限公司 | A kind of preparation method of light stability polyurethane rigid foam plastic |
| CN106928421A (en) * | 2017-04-13 | 2017-07-07 | 合肥科天水性科技有限责任公司 | A kind of clothing leather soft bed material and preparation method thereof |
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Application publication date: 20120418 |