CN105688851A - Preparation method of amino polysilsesquioxane p-aramid fiber composite adsorption material - Google Patents

Preparation method of amino polysilsesquioxane p-aramid fiber composite adsorption material Download PDF

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CN105688851A
CN105688851A CN201610166222.XA CN201610166222A CN105688851A CN 105688851 A CN105688851 A CN 105688851A CN 201610166222 A CN201610166222 A CN 201610166222A CN 105688851 A CN105688851 A CN 105688851A
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aramid fiber
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amino
polysilsesquioxane
fiber composite
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CN105688851B (en
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曲荣君
王孕峰
张盈
孙昌梅
潘方伟
贾欣桦
纪春暖
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Ludong University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26—Synthetic macromolecular compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
    • B01J2220/4893—Residues derived from used synthetic products, e.g. rubber from used tyres

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Abstract

By aiming at the problem of difficult recovery and utilization of the existing polysilsesquioxane after heavy metal adsorption and the problem of difficult reutilization of waste aramid fiber, the invention provides a preparation method of an amino polysilsesquioxane p-aramid fiber composite adsorption material. The method has the beneficial effects that the amino polysilsesquioxane p-aramid fiber composite adsorption material obtained through preparation can improve the utilization rate of an adsorption agent for adsorbing functional groups, and can increase the specific surface area of an adsorbing agent and a solution containing heavy metal ions, so that the adsorption quantity is increased; meanwhile, after the polysilsesquioxane adsorbing agent adsorbs heavy metals, the extraction and the recovery become easy; meanwhile, the chemical properties of the adsorbing agents become more stable; meanwhile, the reutilization of the waste aramid fiber resource is realized; the environment problem caused by heavy metal pollution can be solved.

Description

A kind of preparation method of amino polysilsesquioxane para-aramid fiber composite adsorbing material
Technical field
The preparation method that the present invention relates to a kind of adsorbent, the preparation method particularly relating to a kind of composite adsorbing material, belong to adsorbing material technical field。
Background technology
So-called heavy metal refers to the proportion metal more than 5, heavy metal pollution such as water pollution, soil pollution, animals and plants can be caused damage, the heavy metal of trace can be gathered in human body, liver kidney and other organs being caused damage, the method processing heavy metal pollution at present mainly has chelating resin method, the sedimentation method, polymer chelating agent method, membrane separation technique, activated carbon adsorption, natural zeolite absorption method, ion exchange etc.。Using adsorbent to carry out Adsorption of Heavy Metal Ions, adsorbance is high, and selectivity is good, and the rate of adsorption is increasingly becoming the focus of research soon。
Polysilsesquioxane containing adsorption function base is as adsorbent, and adsorbance is high, and inexpensively, efficiently, the rate of adsorption is fast, stable chemical nature, is always up the hot topic as adsorbent research。But after granular polysilsesquioxane adsorbent heavy metal, it is difficult to recycling, siliconoxygen bond internal crosslinking can be covered adsorption function base simultaneously, makes the area of adsorption function group contacts solution reduce, makes the utilization rate of adsorption function base reduce。
Aramid fiber is as a kind of emerging macromolecular material, have in space flight and aviation and military project etc. and be widely applied very much, it is extensive that simultaneous aramid fiber is applied, some discarded aramid fibers also produce therewith, owing to aramid fiber is heat-resist, acid-fast alkali-proof, corrosion-resistant, conventional method is difficult to process, processing now the topmost method of aramid fiber is landfill, therefore can using the discarded aramid fiber adsorbent as process heavy metal pollution, play its corrosion resistant effect, make adsorbent heavy metal ion become easily to extract easily to reclaim simultaneously, the problem simultaneously solving discarded aramid fiber recycling。
Thus amino polysilsesquioxane and both aramid fibers are combined, prepare amino polysilsesquioxane para-aramid fiber composite adsorbing material, the utilization rate of adsorption function group can either be improved, improve adsorbance simultaneously, fibrous adsorbent also is able to better recycle heavy metal resources, and discarded aramid fiber can be better profited from, it is possible to solve heavy metal pollution problem well, it is achieved resource reclaim recycles。
Summary of the invention
The recycling problem of problem and the discarded aramid fiber recycled it is difficult to, it is provided that the preparation method of a kind of amino polysilsesquioxane para-aramid fiber composite adsorbing material after the present invention is directed to existing polysilsesquioxane Adsorption of Heavy Metals。
The technical scheme is that
The preparation method of a kind of amino polysilsesquioxane para-aramid fiber composite adsorbing material, it is characterised in that comprise the steps:
1) by para-aramid fiber respectively with toluene, acetone and ethanolic extraction, dry；
2) being mixed with anhydrous dimethyl sulphoxide by NaH under nitrogen protection, at 60～70 DEG C, stirring reaction is to after becoming clear solution, cooling；
3) to step 2) gained solution adds step 1) para-aramid fiber of gained, the mol ratio of described NaH and para-aramid fiber is 1:1～1:10, stir at 25～30 DEG C, aramid fiber surface is metallized, epoxychloropropane generation substitution reaction it is added thereto to after 6～12 hours, the mol ratio of described epoxychloropropane and NaH is 1:1, after having reacted, products obtained therefrom ethanolic extraction post-drying is obtained product I；
4) by step 3 under nitrogen protection) products obtained therefrom I mixes with amino silicane coupling agent; dimethyl sulfoxide is solvent; described amino silicane coupling agent and step 2) in the mol ratio of NaH be 1:1～10:1; stirring reaction at 60～80 DEG C, obtains product II by products obtained therefrom ethanolic extraction post-drying；
5) by step 4 under nitrogen protection) products obtained therefrom II mixes with amino silicane coupling agent; dimethyl sulfoxide is solvent; described amino silicane coupling agent and step 2) in the mol ratio of NaH be 1:1～16:1; stirring reaction at 60 DEG C; products obtained therefrom adopts sol-gel process to be hydrolyzed polymerization; then ageing, uses dehydrated alcohol extracting, dries to obtain amino polysilsesquioxane para-aramid fiber composite adsorbing material。
Further, step 5) described in sol-gel process specifically comprise the following steps that the NH of 0.014g/ml being added dropwise over 4～6ml in stirring downhill reaction products obtained therefrom4F solution, stops continuing after heat release stirring 24 hours until solution。
Further, step 5) described in ageing process as follows: digestion time 7～12 days, temperature 60～80 DEG C。
Further, step 4) and 5) described in amino silicane coupling agent be the one in 3-TSL 8330, APTES or 3-amino propyl methyl diethoxy silane。
Further, step 3) in response time of substitution reaction be 12～24 hours。
Further, step 4) described in response time be 12～48 hours。
Further, step 5) described in response time be 6～12 hours。
The present invention is also claimed the polysilsesquioxane para-aramid fiber composite adsorbing material and the application in Adsorption of Heavy Metals field of the above-mentioned composite adsorbing material that adopt above-mentioned preparation method to prepare。
The invention has the beneficial effects as follows:
1) compared with block polysilsesquioxane, largely avoid the internal crosslinking of polysilsesquioxane siliconoxygen bond, the amino polysilsesquioxane para-aramid fiber composite adsorbing material prepared can improve the utilization rate of adsorbent function base, increase the specific surface area that adsorbent contacts with the solution containing heavy metal ion, thus improving adsorbance；
2) become after polysilsesquioxane adsorbent heavy metal can be made easily to extract easily to reclaim, make the chemical property of adsorbent become more stable simultaneously, be simultaneously achieved the recycling of discarded aramid fiber resource, solve the environmental problem that heavy metal pollution causes。
Accompanying drawing explanation
Fig. 1 is the infrared spectrum of para-aramid fiber and embodiment 1 products obtained therefrom；
Fig. 2 is para-aramid fiber scanning electron microscopic picture；
Fig. 3 is the scanning electron microscopic picture of embodiment 2 products obtained therefrom；
Fig. 4 is the scanning electron microscopic picture of embodiment 3 products obtained therefrom；
Fig. 5 is the scanning electron microscopic picture of embodiment 4 products obtained therefrom；
Fig. 6 is the scanning electron microscopic picture of embodiment 5 products obtained therefrom；
Fig. 7 is each embodiment products obtained therefrom adsorption effect schematic diagram to different heavy metal ion；
In Fig. 1, line 1 is the infrared spectrum of para-aramid fiber；Line 2 is the infrared spectrum of embodiment 1 products obtained therefrom。
Detailed description of the invention
Below in conjunction with example, principles of the invention and feature being described, example is served only for explaining the present invention, is not intended to limit the scope of the present invention。
Embodiment 1:
1) para-aramid fiber is put in apparatus,Soxhlet's, successively with toluene, acetone, ethanolic extraction 24 hours, be placed in the baking oven of 60 DEG C and dry；
2) by after inflated with nitrogen lasting in the there-necked flask of 250ml 5 minutes, NaH powder 0.4054g (17mmol) is added in there-necked flask, it is added thereto to 150ml dimethyl sulfoxide (2100mmol) subsequently, it is warming up under 70 DEG C of stirring conditions and reacts 50 minutes, become, after clear pale yellow color solution, being cooled to 30 DEG C until solution；
3) to step 2) gained solution adds 4g step 1) para-aramid fiber of gained, the mol ratio of para-aramid fiber and NaH is 1:1, it is added thereto to 1.3ml epoxychloropropane generation substitution reaction after reacting 6 hours under 30 DEG C of conditions, the mol ratio of epoxychloropropane and NaH is 1:1, continue products obtained therefrom ethanolic extraction 24 hours after reaction 24 hours, be placed in baking oven and dry to obtain product I；
4) product I is joined in the there-necked flask of 250ml of full nitrogen, the dimethyl sulfoxide solvent of 150ml and the 3-TSL 8330 of 3g is added in flask, the mol ratio of 3-TSL 8330 and NaH is 1:1, stirring reaction 48 hours at 60 DEG C, by products obtained therefrom ethanolic extraction 24 hours, it is placed in baking oven and dries to obtain product II；
5) in the 250ml there-necked flask of full nitrogen, add the dimethyl sulfoxide solvent of 120ml, the 3-TSL 8330 of product II and 30g is added in flask, the mol ratio of 3-TSL 8330 and NaH is 10:1, stirring reaction 12 hours at 60 DEG C, take out gained solution and fiber is placed in beaker, be added thereto to the NH of 0.014g/ml4Stirring 24 hours is continued after F solution 5ml, it is transferred in polypropylene vial by reactant and solvent under 80 DEG C of conditions ageing 7 days afterwards, aramid fiber is taken out, with dehydrated alcohol extracting 80 hours, is placed in vacuum drying oven and dries to obtain amino polysilsesquioxane para-aramid fiber composite。
Embodiment 2:
1) para-aramid fiber is put in apparatus,Soxhlet's, successively with toluene, acetone, ethanolic extraction 24 hours, be placed in the baking oven of 60 DEG C and dry；
2) by after inflated with nitrogen lasting in the there-necked flask of 250ml 5 minutes, NaH powder 0.4054g (17mmol) is added in there-necked flask, it is added thereto to 100ml dimethyl sulfoxide (1400mmol) subsequently, it is warming up under 70 DEG C of stirring conditions and reacts 50 minutes, become, after clear pale yellow color solution, being cooled to 30 DEG C until solution；
3) to step 2) gained solution adds 8g step 1) para-aramid fiber of gained, the mol ratio of para-aramid fiber and NaH is 2:1, the epoxychloropropane generation substitution reaction of 1.3ml it is added thereto to after reacting 8 hours under 30 DEG C of conditions, the mol ratio of epoxychloropropane and NaH is 1:1, continue products obtained therefrom ethanolic extraction 24 hours after reaction 12 hours, be placed in baking oven and dry to obtain product I；
4) product I is joined in the there-necked flask of 250ml of full nitrogen, the dimethyl sulfoxide solvent of 150ml and the 3-TSL 8330 of 6g is added in flask, the mol ratio of 3-TSL 8330 and NaH is 2:1, stirring reaction 36 hours at 70 DEG C, by products obtained therefrom ethanolic extraction 24 hours, it is placed in baking oven and dries to obtain product II；
5) in the 250ml there-necked flask of full nitrogen, add the dimethyl sulfoxide solvent of 120ml, backward flask in add the 3-TSL 8330 of product II and 15g, the mol ratio of 3-TSL 8330 and NaH is 5:1, stirring reaction 8 hours under 60 DEG C of conditions, take out gained solution and fiber is placed in beaker, be added thereto to the NH of 0.014g/ml4Stirring 24 hours is continued after F solution 5ml, it is transferred in polypropylene vial by reactant and solvent under 70 DEG C of conditions ageing 9 days afterwards, aramid fiber is taken out, with dehydrated alcohol extracting 80 hours, is placed in vacuum drying oven and dries to obtain amino polysilsesquioxane para-aramid fiber composite。
Embodiment 3:
1) para-aramid fiber is put in apparatus,Soxhlet's, successively with toluene, acetone, ethanolic extraction 24 hours, be placed in the baking oven of 60 DEG C and dry；
2) by after inflated with nitrogen lasting in the there-necked flask of 250ml 5 minutes, NaH powder 0.4054g (17mmol) is added in there-necked flask, it is added thereto to 200ml dimethyl sulfoxide (2800mmol) subsequently, it is warming up under 70 DEG C of stirring conditions and reacts 50 minutes, become, after clear pale yellow color solution, being cooled to 30 DEG C until solution；
3) to step 2) gained solution adds 40g step 1) para-aramid fiber of gained, the mol ratio of para-aramid fiber and NaH is 10:1, the epoxychloropropane generation substitution reaction of 1.3ml it is added thereto to after reacting 10 hours under 30 DEG C of conditions, the mol ratio of epoxychloropropane and NaH is 1:1, continue products obtained therefrom ethanolic extraction 24 hours after reaction 18 hours, be placed in baking oven and dry to obtain product I；
4) product I is joined in the there-necked flask of 250ml of full nitrogen, the dimethyl sulfoxide solvent of 150ml and the APTES of 15g is added in flask, the mol ratio of APTES and NaH is 5:1, stirring reaction 24 hours at 75 DEG C, by products obtained therefrom ethanolic extraction 24 hours, it is placed in baking oven and dries to obtain product II；
5) in the 250ml there-necked flask of full nitrogen, add the dimethyl sulfoxide solvent of 120ml, backward flask in add the APTES of product II and 39g, the mol ratio of APTES and NaH is 13:1, stirring reaction 6 hours under 60 DEG C of conditions, take out gained solution and fiber is placed in beaker, be added thereto to the NH of 0.014g/ml4Stirring 24 hours is continued after F solution 6ml, it is transferred in polypropylene vial by reactant and solvent under 75 DEG C of conditions ageing 8 days afterwards, aramid fiber is taken out, with dehydrated alcohol extracting 80 hours, is placed in vacuum drying oven and dries to obtain amino polysilsesquioxane para-aramid fiber composite。
Embodiment 4:
1) para-aramid fiber is put in apparatus,Soxhlet's, successively with toluene, acetone, ethanolic extraction 24 hours, be placed in the baking oven of 60 DEG C and dry；
2) by after inflated with nitrogen lasting in the there-necked flask of 250ml 5 minutes, NaH powder 0.4054g (17mmol) is added in there-necked flask, it is added thereto to 150ml dimethyl sulfoxide (2100mmol) subsequently, it is warming up under 70 DEG C of stirring conditions and reacts 50 minutes, become, after clear pale yellow color solution, being cooled to 25 DEG C until solution；3) to step 2) gained solution adds 20g step 1) para-aramid fiber of gained, the mol ratio of para-aramid fiber and NaH is 5:1, it is added thereto to 1.3ml epoxychloropropane generation substitution reaction after reacting 12 hours under 25 DEG C of conditions, the mol ratio of epoxychloropropane and NaH is 1:1, continue products obtained therefrom ethanolic extraction 24 hours after reaction 20 hours, be placed in baking oven and dry to obtain product I；
4) product I is joined in the there-necked flask of 250ml of full nitrogen, the dimethyl sulfoxide solvent of 150ml and the APTES of 21g is added in flask, the mol ratio of APTES and NaH is 7:1, stirring reaction 30 hours at 80 DEG C, by products obtained therefrom ethanolic extraction 24 hours, it is placed in baking oven and dries to obtain product II；
5) in the 250ml there-necked flask of full nitrogen, add the dimethyl sulfoxide solvent of 120ml, backward flask in add the APTES of product II and 3g, the mol ratio of APTES and NaH is 1:1, stirring reaction 12 hours under 60 DEG C of conditions, take out gained solution and fiber is placed in beaker, be added thereto to the NH of 0.014g/ml4Stirring 24 hours is continued after F solution 4ml, it is transferred in polypropylene vial by reactant and solvent under 60 DEG C of conditions ageing 12 days afterwards, aramid fiber is taken out, with dehydrated alcohol extracting 80 hours, is placed in vacuum drying oven and dries to obtain amino polysilsesquioxane para-aramid fiber composite。
Embodiment 5:
1) para-aramid fiber is put in apparatus,Soxhlet's, successively with toluene, acetone, ethanolic extraction 24 hours, be placed in the baking oven of 60 DEG C and dry；
2) by after inflated with nitrogen lasting in the there-necked flask of 250ml 5 minutes, in there-necked flask, add the NaH powder of 0.4054g, be added thereto to 150ml dimethyl sulfoxide subsequently, be warming up under 70 DEG C of stirring conditions and react 50 minutes, become, after clear pale yellow color solution, being cooled to 30 DEG C until solution；
3) to step 2) gained solution adds 15g step 1) para-aramid fiber of gained, the mol ratio of para-aramid fiber and NaH is 5:1, the epoxychloropropane generation substitution reaction of 1.3ml it is added thereto to after reacting 12 hours under 30 DEG C of conditions, the mol ratio of epoxychloropropane and NaH is 1:1, continue products obtained therefrom ethanolic extraction 24 hours after reaction 24 hours, be placed in baking oven and dry to obtain product I；
4) product I is joined in the there-necked flask of 250ml of full nitrogen, the dimethyl sulfoxide solvent of 150ml and the 3-amino propyl methyl diethoxy silane of 30g is added in flask, the mol ratio of 3-amino propyl methyl diethoxy silane and NaH is 10:1, stirring reaction 48 hours at 65 DEG C, by products obtained therefrom ethanolic extraction 24 hours, it is placed in baking oven and dries to obtain product II；
5) in the 250ml there-necked flask of full nitrogen, add the dimethyl sulfoxide solvent of 120ml, backward flask in add the 3-amino propyl methyl diethoxy silane of product II and 48g, the mol ratio of 3-amino propyl methyl diethoxy silane and NaH is 16:1, stirring reaction 12 hours at 60 DEG C, take out gained solution and fiber is placed in beaker, be added thereto to the NH of 0.014g/ml4Stirring 24 hours is continued after F solution 5ml, it is transferred in polypropylene vial by reactant and solvent under 65 DEG C of conditions ageing 12 days afterwards, aramid fiber is taken out, with dehydrated alcohol extracting 80 hours, is placed in vacuum drying oven and dries to obtain amino polysilsesquioxane para-aramid fiber composite。
The concrete operation step of the testing adsorption effect of embodiment 1～5 products obtained therefrom is as follows:
Weigh five kinds of adsorbing materials 1,2,3,4,5 that quality is the above-mentioned gained of 20mg respectively, in tool plug conical flask, respectively add 5 × 10-3The Cu (II) of mol/L, Hg (II), Ag (I) and Pb (II) and 1 × 10-3The aqueous solution 20mL of the Au (III) of mol/L, is placed in gas bath agitator and vibrates 24 hours。By the concentration of residual metallic ion in Solution by Atomic Absorption Spectrophotometry。Calculate the adsorbance Q (mmol/g) of adsorbing material with formula (1), its adsorption effect is as shown in Figure 6。
Q = ( C 0 - C e ) V W - - - ( 1 )
Wherein Q: the adsorbance (mmol/g) of heavy metal ion；C0: ion concentration (mmol/mL) initial in solution；Ce: the concentration (mmol/mL) of effects of ion after adsorbent balance；V: the volume (mL) of solution；W: adsorbent mass (g)。
Fig. 1 is the infrared spectrum of the adsorbent of para-aramid fiber and embodiment 1 preparation, and compared with para-aramid fiber, prepared adsorbent is at 3400cm-1The absworption peak of left and right broadens and is primarily due to amido link N-H stretching vibration peak and what silicone hydroxyl stretching vibration caused, at 2925cm-1Place occurs in that absworption peak is the CH being connected with Si2Infrared absorption peak, adsorbent is at 1637cm-1The infrared absorption peak absorption intensity of left and right strengthens, and is because not only having C=O stretching vibration peak herein, is also SiO2The common exercising result of stretching vibration, simultaneously at 1042cm-1Place occurs in that SiO2Characteristic absorption peak。
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all within the spirit and principles in the present invention, any amendment of making, equivalent replacement, improvement etc., should be included within protection scope of the present invention。

Claims (9)

1. the preparation method of an amino polysilsesquioxane para-aramid fiber composite adsorbing material, it is characterised in that comprise the steps:
1) by para-aramid fiber respectively with toluene, acetone and ethanolic extraction, dry；
2) being mixed with anhydrous dimethyl sulphoxide by NaH under nitrogen protection, at 60～70 DEG C, stirring reaction is to after becoming clear solution, cooling；
3) to step 2) gained solution adds step 1) para-aramid fiber of gained, the mol ratio of described NaH and para-aramid fiber is 1:1～1:10, stir at 25～30 DEG C, aramid fiber surface is metallized, epoxychloropropane generation substitution reaction it is added thereto to after 6～12 hours, the mol ratio of described epoxychloropropane and NaH is 1:1, after having reacted, products obtained therefrom ethanolic extraction post-drying is obtained product I；
4) by step 3 under nitrogen protection) products obtained therefrom I mixes with amino silicane coupling agent; dimethyl sulfoxide is solvent; described amino silicane coupling agent and step 2) in the mol ratio of NaH be 1:1～10:1; stirring reaction at 60～80 DEG C, obtains product II by products obtained therefrom ethanolic extraction post-drying；
5) by step 4 under nitrogen protection) products obtained therefrom II mixes with amino silicane coupling agent; dimethyl sulfoxide is solvent; described amino silicane coupling agent and step 2) in the mol ratio of NaH be 1:1～16:1; stirring reaction at 60 DEG C; products obtained therefrom adopts sol-gel process to be hydrolyzed polymerization; then ageing, uses dehydrated alcohol extracting, dries to obtain amino polysilsesquioxane para-aramid fiber composite adsorbing material。
2. the preparation method of amino polysilsesquioxane para-aramid fiber composite adsorbing material according to claim 1, it is characterized in that, step 5) described in sol-gel process specifically comprise the following steps that the NH of 0.014g/ml being added dropwise over 4～6ml in stirring downhill reaction products obtained therefrom4F solution, stops continuing after heat release stirring 24 hours until solution。
3. the preparation method of amino polysilsesquioxane para-aramid fiber composite adsorbing material according to claim 1, it is characterised in that step 5) described in ageing process as follows: digestion time 7～12 days, temperature 60～80 DEG C。
4. the preparation method of amino polysilsesquioxane para-aramid fiber composite adsorbing material according to claim 1, it is characterized in that, step 4) and 5) described in amino silicane coupling agent be the one in 3-TSL 8330, APTES or 3-amino propyl methyl diethoxy silane。
5. the preparation method of amino polysilsesquioxane para-aramid fiber composite adsorbing material according to claim 1, it is characterised in that step 3) in response time of substitution reaction be 12～24 hours。
6. the preparation method of amino polysilsesquioxane para-aramid fiber composite adsorbing material according to claim 1, it is characterised in that step 4) described in response time be 12～48 hours。
7. the preparation method of amino polysilsesquioxane para-aramid fiber composite adsorbing material according to claim 1, it is characterised in that step 5) described in response time be 6～12 hours。
8. the amino polysilsesquioxane para-aramid fiber composite adsorbing material that prepared by the preparation method as according to any one of claim 1-7。
9. the amino polysilsesquioxane para-aramid fiber composite adsorbing material according to claim 8 application in Adsorption of Heavy Metals。
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CN109694522A (en) * 2017-10-20 2019-04-30 中国石油化工股份有限公司 Low VOC Low-odor polypropylene resin composition and preparation method thereof

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