CN102418276A - Preparation method of flame-retardant waterborne polyurethane - Google Patents
Preparation method of flame-retardant waterborne polyurethane Download PDFInfo
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- CN102418276A CN102418276A CN2011103378812A CN201110337881A CN102418276A CN 102418276 A CN102418276 A CN 102418276A CN 2011103378812 A CN2011103378812 A CN 2011103378812A CN 201110337881 A CN201110337881 A CN 201110337881A CN 102418276 A CN102418276 A CN 102418276A
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Abstract
The invention discloses a preparation method of flame-retardant waterborne polyurethane. The preparation method comprises the following steps of: a. adding methyl-isobutyl ketone, MDI (Diphenylmethane Diisocyanate) and a catalytic amount of dibutyltion dilaurate in a reaction kettle filled with inert gases and heating and dissolving by stirring; b. dripping polyether polyol (PPG) and hydroxyl acrylic ester and controlling the temperature and reacting for 1-5 hours to obtain a prepolymerization product; c. adding 1,2,4-triazole and dihydroxy trimethylacetic acid end-capping reagents and reacting for 1-2 hours; d. adding triethylamine as a neutralizing agent to obtain the end-capped polyurethane; e. removing the methyl-isobutyl ketone as a solvent at the reduced pressure; f. adding deionized water to obtain water aqua with the solid content of 30-35 percent; and g. adding a flame retardant for stirring at high speed to enable the flame retardant to be fully dispersed and obtain the flame-retardant waterborne polyurethane. The flame-retardant waterborne polyurethane obtained in the invention has the advantages of stronger compound function, favorable cross-linking property and water resistance, high oxygen index, favorable flame-resisting performance, favorable compound collaborative performance and stable storage performance.
Description
Technical field:
The present invention relates to a kind of flame-retardant aqueous polyurethane, particularly a kind of preparation method of flame-retardant aqueous polyurethane.
Background technology:
In recent years, along with the raising of social progress and living standards of the people, all kinds of civilian and consumption figures fabrics for industrial use increase sharply, and the fire resistance that improves textiles is to guaranteeing safety and reducing fire incident extremely important realistic meaning is arranged.Flame-retardant textile is mainly used in protective clothing: Work Clothes and military uniforms such as fire-fighting, stokehold, welder; General clothes: clothes such as nightwear, infant; Family decoration: carpet, curtain, wall paper etc.; Use on the bed: woollen blanket, bedcover etc.; Furniture is used: chair cover, the tablecloth etc.; Communications and transportation is used: buntings such as car, ship, aircraft; Military using: gun cover, tent cloth etc.; Industrial: filter cloth etc.; The public place is used: cinema curtain etc.; Other: wig, Fake Furs, woolen toy etc.Flame retardant textiles will have market widely at home and abroad.China's flame-retarded technology and fire retardant development are comparatively slow, and research fire retardant and flame-retarded technology have become crucial problem.
Utilize the performance that the polyurethane film-forming ability is strong and can give fabric elasticity; Have anti-preferably rubbing property and feel after can making the fabric coating flame-proof treatment; Make polyurethane latex produce absorption or coating effect through special manufacture craft to the ultra-fine grain of flame-retardant composition; Thereby the fire retardant particle can evenly be distributed and be tightly adhered in the polyurethane film of fabric face, reached comparatively ideal effect.
Summary of the invention:
Goal of the invention:, the invention provides a kind of preparation method of flame-retardant aqueous polyurethane to the defective that prior art exists.
Technical scheme: for realizing the foregoing invention purpose, the present invention adopts following technical scheme:
A kind of preparation method of flame-retardant aqueous polyurethane may further comprise the steps: a, in being full of the agitated reactor of inert gas, add the dibutyl tin laurate of organic solvent methyl iso-butyl ketone (MIBK), MDI and catalytic amount, stir that 60 ℃ of dissolvings of heating are for use down; B, in the solution that step a obtains, drip PPG PPG and hydroxy acrylate, temperature control reaction 1 ~ 5h obtains prepolymer product; C, in step b, obtain to add in the prepolymer product end-capping reagent 1,2,4-triazole and dihydroxy pivalic acid react 1 ~ 2h; D, add the neutralizer triethylamine, obtain the polyurethane of end-blocking; E, decompression remove the solvent methyl iso-butyl ketone (MIBK); F, add deionized water, it is 30 ~ 35% aqueous polyurethane that reactant liquor is mixed with solid content; G, dispersion at last add fire retardant diethyl-N-double hydroxyethyl-aminomethyl phosphonic acid ester, can obtain product, and wherein, the mass ratio of fire retardant and blocked polyurethane solid content is 1:1 ~ 30.
The mass ratio of said MDI and PPG is 1 ~ 3:1.
According to above technical scheme, can realize following beneficial effect: compared with prior art, the present invention has the following advantages: flame-retardant aqueous polyurethane that the present invention obtains; Have stronger complex function, oxygen index (OI) is high, and flame resistance can be good; The composite concertedness of product is good, stable storing.
The specific 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:
In the agitated reactor that is full of nitrogen or other inert gas, add successively organic solvent methyl iso-butyl ketone (MIBK) (85.0kg) and MDI (1.0kmol, 254.0kg), two laurate diisobutyl tin (1.2kg) of catalytic amount are heated to 60 ℃ of dissolvings under stirring; In agitated reactor, drip PPG PPG (235.0kg) and hydroxy acrylate (10.5kg), the control temperature is dripped and is finished insulation reaction 1 ~ 5h at 60 ~ 95 ℃; Reactant liquor is warming up to 90 ~ 95 ℃, adds end-capping reagent 1,2,4-triazole (100.0kg) and dihydroxy pivalic acid (25.0kg); Reaction 1 ~ 2h then is cooled to 80 ℃ with reactant liquor, adds the triethylamine neutralizer, obtains the polyurethane of end-blocking; Decompression removes the solvent methyl iso-butyl ketone (MIBK), and adding deionized water, to be mixed with solid content be 30 ~ 35% aqua, takes by weighing fire retardant diethyl-N-double hydroxyethyl-aminomethyl phosphonic acid ester (78.0kg); Add in the aqua, high-speed stirred is even, obtains the composite product of water-based.
Claims (2)
1. the preparation method of a flame-retardant aqueous polyurethane; It is characterized in that; May further comprise the steps: a, in being full of the agitated reactor of inert gas, add the dibutyl tin laurate of organic solvent methyl iso-butyl ketone (MIBK), MDI and catalytic amount, stir that 60 ℃ of dissolvings of heating are for use down; B, in the solution that step a obtains, drip PPG PPG and hydroxy acrylate, temperature control reaction 1 ~ 5h obtains prepolymer product; C, in step b, obtain to add in the prepolymer product end-capping reagent 1,2,4-triazole and dihydroxy pivalic acid react 1 ~ 2h; D, add the neutralizer triethylamine, obtain the polyurethane of end-blocking; E, decompression remove the solvent methyl iso-butyl ketone (MIBK); F, add deionized water, it is 30 ~ 35% aqueous polyurethane that reactant liquor is mixed with solid content; G, dispersion at last add fire retardant diethyl-N-double hydroxyethyl-aminomethyl phosphonic acid ester, can obtain product, and wherein, the mass ratio of fire retardant and blocked polyurethane solid content is 1:1 ~ 30.
2. according to the preparation method of the said flame-retardant aqueous polyurethane of claim 1, it is characterized in that: the mass ratio of said MDI and PPG is 1 ~ 3:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103378812A CN102418276A (en) | 2011-11-01 | 2011-11-01 | Preparation method of flame-retardant waterborne polyurethane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103378812A CN102418276A (en) | 2011-11-01 | 2011-11-01 | Preparation method of flame-retardant waterborne polyurethane |
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| Publication Number | Publication Date |
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| CN102418276A true CN102418276A (en) | 2012-04-18 |
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| CN2011103378812A Pending CN102418276A (en) | 2011-11-01 | 2011-11-01 | Preparation method of flame-retardant waterborne polyurethane |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104497268A (en) * | 2014-11-28 | 2015-04-08 | 苏州市安特菲尔新材料有限公司 | Flame-retardant conducting polyurethane material and preparation method thereof |
| CN107474526A (en) * | 2017-09-07 | 2017-12-15 | 绵阳旺通科技有限公司 | A kind of preparation method for compounding the good flame-retardant polyurethane of concertedness |
| CN109400846A (en) * | 2018-10-27 | 2019-03-01 | 濮阳天健生物科技有限公司 | A kind of chemical reaction kettle composite insulation boards and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1760224A (en) * | 2005-09-29 | 2006-04-19 | 上海申真企业发展有限公司 | Method for preparing inflaming retarding type copolymerization latex of urethane acrylate |
| CN101440153A (en) * | 2008-12-09 | 2009-05-27 | 东华大学 | Preparation of aqueous polyurethane fluid dispersion used with expansion type flame retardant |
-
2011
- 2011-11-01 CN CN2011103378812A patent/CN102418276A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1760224A (en) * | 2005-09-29 | 2006-04-19 | 上海申真企业发展有限公司 | Method for preparing inflaming retarding type copolymerization latex of urethane acrylate |
| CN101440153A (en) * | 2008-12-09 | 2009-05-27 | 东华大学 | Preparation of aqueous polyurethane fluid dispersion used with expansion type flame retardant |
Non-Patent Citations (3)
| Title |
|---|
| 周向东等: "封端型水系聚氨酯复合阻燃剂的研制及应用", 《湖南工程学院学报》 * |
| 洪哲等: "直接氧化法制备羟基特戊酸的研究", 《丹东纺专学报》 * |
| 陈鹤等: "阻燃水性聚氨酯研究进展", 《高分子材料科学与工程》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104497268A (en) * | 2014-11-28 | 2015-04-08 | 苏州市安特菲尔新材料有限公司 | Flame-retardant conducting polyurethane material and preparation method thereof |
| CN104497268B (en) * | 2014-11-28 | 2017-07-14 | 苏州市安特菲尔新材料有限公司 | A kind of flame-retardant conductive polyurethane material and preparation method thereof |
| CN107474526A (en) * | 2017-09-07 | 2017-12-15 | 绵阳旺通科技有限公司 | A kind of preparation method for compounding the good flame-retardant polyurethane of concertedness |
| CN109400846A (en) * | 2018-10-27 | 2019-03-01 | 濮阳天健生物科技有限公司 | A kind of chemical reaction kettle composite insulation boards and preparation method thereof |
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Application publication date: 20120418 |