CN101565895A - Preparation method of coupling agent containing flexible chain macromolecule for waste sisal fibre - Google Patents
Preparation method of coupling agent containing flexible chain macromolecule for waste sisal fibre Download PDFInfo
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- CN101565895A CN101565895A CNA2009101140361A CN200910114036A CN101565895A CN 101565895 A CN101565895 A CN 101565895A CN A2009101140361 A CNA2009101140361 A CN A2009101140361A CN 200910114036 A CN200910114036 A CN 200910114036A CN 101565895 A CN101565895 A CN 101565895A
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Abstract
The invention discloses a preparation method of coupling agent containing flexible chain macromolecule for waste sisal fibre. The method includes the steps of: placing 90-110ml of 1mol/L polyethylene glycol into 1000ml three-mouth flask, heating in oil bath at 90-150 DEG C, then vacuumizing for 0.5-3 hours, and then cooling to 30-70 DEG C. Filling with N2 and adding 90-110ml of 2mol/L toluene diisocyanate, heat preserving in oil bath at 30-80 DEG C with protection of N2, and stirring for 4-10 hours of reaction. And then slowly dropping mixture containing 90-110ml of 2mol/L 3-amino-triethoxysilane and 100-1000ml of analytical pure acetone, reacting until -NCO is completed, vacuumizing and removing acetone. The preparation method provided by the invention has advantages of low production cost, free of pollution, good modified effect for waste sisal fibre, and high intensity shock-resisting ability of wood plastic composite decorative plate prepared by mixing waste sisal fibre treated by the product provided by the invention and polypropylene, and easy processing.
Description
Technical field
The present invention relates to a kind of preparation method of coupling agent containing flexible chain macromolecule for waste sisal fibre.
Background technology
In recent years, because becoming increasingly conspicuous of global energy and environmental problem adopts the resin composite materials of the alternative synthetic fiber enhancing of the abundant natural plant fibre of nature to be subjected to people's attention gradually.Compare with traditional synthetic fiber, that natural plant fibre has is inexpensive, aboundresources, recyclable, degradable, advantage such as renewable, and have strength and stiffness of general fiber, insulation, heat insulation, and proportion is less, the characteristics that specific strength, specific stiffness are all higher are so be that the composite that strengthens base has good performance equally with the natural plant fibre.Sisal fiber also has the incomparable advantage of other fiber except that the characteristic with other natural fabric, hard as quality, density is little, nontoxic, high strength, high-modulus, high resilience, TENSILE STRENGTH height, rub resistance, characteristics such as low temperature resistant.In addition, also have long, the multifrequency natures such as color and luster is pure white, seawater corrosion resistance of fiber, can be through the seawater long period of soaking and not perishable.For a long time, sisal fiber is mainly used in makes sisal hemp yarn, sisal hemp rope, sisal hemp cloth etc., to sisal fiber utilize level lower, surcharge is not high, its new Application Areas is demanded further exploitation urgently.And the leftover pieces of these products then seldom are recycled, and are by burning disposal mostly, and this not only causes the significant wastage of resource, have also aggravated the pollution to environment simultaneously.Therefore, the useless sisal fiber of development and use prepares all kinds of decorating material boards with good cost performance, has important theoretical research and is worth with actual exploitation.The coupling agent of existing sisal fiber is maleic anhydride, elastomer, silane coupler etc. normally, and the source selectivity of raw material is less, and price is more expensive.
Summary of the invention
The purpose of this invention is to provide a kind of the toughness reinforcing cost of useless sisal hemp is reduced, shock resistance improves, be easy to process, the preparation method of free of contamination environment-friendly type coupling agent containing flexible chain macromolecule for waste sisal fibre.
Concrete steps are:
(1) be the there-necked flask that the polyethylene glycol (PEG) of 1mol/L places 1000ml with 90～110ml molar concentration, oil bath is heated to 90 ℃～150 ℃, vacuumizes then, continues to be cooled to 30 ℃～70 ℃ behind 0.5h～3h.
(2) product that step (1) is made fills N
2And add the toluene di-isocyanate(TDI) that 90～110ml molar concentration is 2mol/L (TDI), at N
2Protection oil bath down is incubated 30 ℃～80 ℃, stirring reaction 4h～10h.Slowly dripping 90～110ml molar concentration then is the amino triethoxysilane (WD-50) of 3-of 2mol/L and the mixture that 100ml～1000ml analyzes pure acetone, reaction to-NCO fully till, vacuumize and remove acetone, promptly get flaxen viscous fluid PEG-[Si (OC
2H
5)
3]
2Macromolecular coupling agent.
Concrete condition of the present invention:
(1) the preparation raw material sources of coupling agent containing flexible chain macromolecule for waste sisal fibre of the present invention are extensive, and production cost is lower, can be used for the high materials such as elastomer of substitute valence.
(2) coupling agent containing flexible chain macromolecule for waste sisal fibre synthesis technique of the present invention is simple, and pollution level is very little, and the useless sisal fiber consumption of modification is few, only for 1～5% of sisal hemp amount, just can reach good toughening effect.
(3) the surface-treated useless sisal fiber of the flexible chain macromolecular coupling agent that makes through the present invention and the wood-plastic decorative board of polypropylene preparation are easy to processing, moulding, the no bubble in surface.Impact strength is by untreated 14.78kJ/m
2Bring up to 22.08kJ/m
2, having improved 49.4%, bending strength is 33.92MPa to the maximum, and the bending modulus maximum reaches 0.956GPa, and heat endurance also increases with polypropylene crystalline rate and degree of crystallinity mutually.
Description of drawings
Fig. 1 is the infrared spectrogram of the macromolecular coupling agent that synthesized of embodiment 2.
Mark among the figure: (a) polyethylene glycol (PEG); (b) toluene di-isocyanate(TDI) (TDI) end-blocking PEG; (c) PEG-[Si (OC2H5) 3] 2.
The specific embodiment
Embodiment 1:
(1) with the 100ml molar concentration be the there-necked flask that the cetomacrogol 1000 of 1mol/L places 1000ml, 100 ℃ of oil bath heating vacuumize then, continue to be cooled to 50 ℃ behind the 0.5h.
(2) product that step (1) is made fills N
2And to add the 100ml molar concentration be the toluene di-isocyanate(TDI) (TDI) of 2mol/L, at N
2Protection oil bath down is incubated 40 ℃; stirring reaction 6h; slowly dripping the 100ml molar concentration then is the amino triethoxysilane (WD-50) of 3-of 2mol/L and the mixture of 300ml acetone (analyzing pure); reaction to-NCO fully till; vacuumize and remove acetone, promptly get flaxen viscous fluid PEG-[Si (OC
2H
5)
3]
2Macromolecular coupling agent.After the flexible macromolecular coupling agent that makes was handled useless sisal hemp, measure with the wood-plastic decorative board of polypropene blended preparation: when consumption was the 1-5% of sisal hemp amount, impact strength was by untreated 14.78kJ/m
2Bring up to 17.55kJ/m
2, bending strength is 30.14MPa, bending modulus reaches 0.951GPa.
Embodiment 2:
(1) with the 100ml molar concentration be the there-necked flask that the Macrogol 6000 of 1mol/L places 1000ml, 120 ℃ of oil bath heating vacuumize then, continue to be cooled to 60 ℃ behind the 1h.
(2) product that step (1) is made fills N
2And to add the 100ml molar concentration be the toluene di-isocyanate(TDI) (TDI) of 2mol/L, at N
2Protection oil bath down is incubated 50 ℃, stirring reaction 8h.Slowly drip the 100ml molar concentration then and be the amino triethoxysilane (WD-50) of 3-of 2mol/L and the mixture that 600ml analyzes pure acetone, reaction to-till NCO is complete, vacuumizes and remove acetone, promptly get flaxen viscous fluid PEG-[Si (OC
2H
5)
3]
2Macromolecular coupling agent.
Fig. 1 is the infrared spectrogram of the macromolecular coupling agent that synthesized, 3507cm in the curve (a)
-1The place is-OH stretching vibration absworption peak～1100cm
-1For-C-O-C stretching vibration absworption peak; (b)～2270cm
-1Stretching vibration be-the NCO absworption peak; 3516,3300cm
-1Stretching vibration be-absworption peak of NH-; (c)～2270cm
-1Absworption peak disappears, illustrate-NCO reacts completely, curve (b) and (c) in, 1721cm
-1Stretching vibration be-absworption peak of C=O.This explanation on the amino triethoxysilane of 3-(WD-50) in the grafting soft segment.After the flexible macromolecular coupling agent that makes was handled useless sisal hemp, measure with the wood-plastic decorative board of polypropene blended preparation: when consumption was the 1-5% of sisal hemp amount, impact strength was by untreated 14.78kJ/m
2Bring up to 22.08kJ/m
2, having improved 49.4%, bending strength is 33.92MPa to the maximum, and the bending modulus maximum reaches 0.956GPa, and heat endurance also increases with polypropylene crystalline rate and degree of crystallinity mutually.
Embodiment 3:
(1) with the 100ml molar concentration be the there-necked flask that the cetomacrogol 1000 0 of 1mol/L places 1000ml, 120 ℃ of oil bath heating vacuumize then, continue to be cooled to 60 ℃ behind the 1h.
(2) product that step (1) is made fills N
2And to add the 100ml molar concentration be the toluene di-isocyanate(TDI) (TDI) of 2mol/L, at N
2Protection oil bath down is incubated 60 ℃; stirring reaction 8h; slowly dripping the 100ml molar concentration then is the amino triethoxysilane (WD-50) of 3-of 2mol/L and the mixture that 800ml analyzes pure acetone; reaction to-NCO fully till; vacuumize and remove acetone, promptly get flaxen viscous fluid PEG-[Si (OC
2H
5)
3]
2Macromolecular coupling agent.After the flexible macromolecular coupling agent that makes was handled useless sisal hemp, measure with the wood-plastic decorative board of polypropene blended preparation: when consumption was the 1-5% of sisal hemp amount, impact strength was by untreated 14.78kJ/m
2Bring up to 19.04kJ/m
2, bending strength is 33.82MPa, bending modulus reaches 0.889GPa.
Claims (1)
1. the preparation method of a coupling agent containing flexible chain macromolecule for waste sisal fibre is characterized in that concrete steps are:
(1) be the there-necked flask that the polyethylene glycol of 1mol/L places 1000ml with 90～110ml molar concentration, oil bath is heated to 90 ℃～150 ℃, vacuumizes then, continues to be cooled to 30 ℃～70 ℃ behind 0.5h～3h;
(2) product that step (1) is made fills N
2And add the toluene di-isocyanate(TDI) that 90～110ml molar concentration is 2mol/L, at N
2Protection oil bath down is incubated 30 ℃～80 ℃, stirring reaction 4h～10h; Slowly dripping 90～110ml molar concentration then is the amino triethoxysilane of 3-of 2mol/L and the mixture that 100ml～1000ml analyzes pure acetone, reaction to-NCO fully till, vacuumize and remove acetone, promptly get coupling agent containing flexible chain macromolecule for waste sisal fibre.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009101140361A CN101565895A (en) | 2009-05-05 | 2009-05-05 | Preparation method of coupling agent containing flexible chain macromolecule for waste sisal fibre |
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|---|---|---|---|
| CNA2009101140361A CN101565895A (en) | 2009-05-05 | 2009-05-05 | Preparation method of coupling agent containing flexible chain macromolecule for waste sisal fibre |
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|---|---|
| CN101565895A true CN101565895A (en) | 2009-10-28 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104313876A (en) * | 2014-10-15 | 2015-01-28 | 四川大学 | Method for modifying natural fibers for anion polymer nylon 6 reaction |
-
2009
- 2009-05-05 CN CNA2009101140361A patent/CN101565895A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104313876A (en) * | 2014-10-15 | 2015-01-28 | 四川大学 | Method for modifying natural fibers for anion polymer nylon 6 reaction |
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Open date: 20091028 |