CN107556637A - A kind of ester modified fire proofing material of silicic acid and preparation method thereof - Google Patents
A kind of ester modified fire proofing material of silicic acid and preparation method thereof Download PDFInfo
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- CN107556637A CN107556637A CN201710973415.0A CN201710973415A CN107556637A CN 107556637 A CN107556637 A CN 107556637A CN 201710973415 A CN201710973415 A CN 201710973415A CN 107556637 A CN107556637 A CN 107556637A
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Abstract
The invention discloses a kind of ester modified fire proofing material of silicic acid, and it is made of the raw material of following weight parts：Dimethyl silicone polymer 34, stannous sulfide 0.1 0.2, esters of silicon acis modified carbon nano-tube 18 20, alkanolamide 12, zinc ricinate 0.3 1, zinc dibutyl dithiocarbamate 0.7 1, pentaerythrite 57, styrene 115 120, ammonium persulfate 34, fire-proof additive 46, stearic acid 12；The esters of silicon acis modified carbon nano-tube that the present invention adds, non-flammable compressive gas can be discharged in burning, effectively reduces oxygen concentration, play good flameproof effect, while it is stable carbon-coating that CNT can be formed in burning, plays good gas phase barriering effect.
Description
Technical field
The invention belongs to Material Field, and in particular to a kind of ester modified fire proofing material of silicic acid and preparation method thereof.
Background technology
Polystyrene foamed material is using polystyrene resin as base-material, adds the auxiliary materials such as foaming agent, heated hair
Steep the light material formed.It has that light, thermal conductivity factor is small, water absorption rate is low, water-fast, ageing-resistant, low temperature resistant, easy processing, valency
The advantages that honest and clean of fine quality, but polystyrene foam heat insulation material, while the life to people brings huge facilitate, its is inflammable
Property also brings certain limitation to its application.Polystyrene foam is combustible material in itself, under fire and hot conditions
Easily decompose and burn and produced with a large amount of poison gases.Therefore, it is badly in need of carrying out pacifying polystyrene foam heat insulation material fire
Research work in terms of full property；And in order to improve the fire protecting performance of sheet material, a variety of inorganic fire-retarded fillers are often added wherein, this
The compatibility of a little fillers and polystyrene is poor, is easily formed and reunited, so as to reduce the mechanical property of finished product；
Therefore, it is an object of the invention to provide a kind of fire proofing material so that various inorganic fillers can have in polystyrene
Disperseing for effect, improves the mechanical property of finished-product material, on the basis of ensureing that mechanical property is higher, has fire prevention resistance well again
Fuel efficiency fruit.
The content of the invention
It is an object of the invention to asking for the difference of the fire-retardant fireproof for polystyrene foam heat insulation material in the prior art
A kind of topic, there is provided ester modified fire proofing material of silicic acid and preparation method thereof.
To achieve the above object, the present invention uses following technical scheme：
A kind of ester modified fire proofing material of silicic acid, it is made of the raw material of following weight parts：
Dimethyl silicone polymer 3-4, esters of silicon acis modified carbon nano-tube 18-20, alkanolamide 1-2, zinc ricinate 0.3-1, two
Zinc dibutyl dithiocarbamate 0.7-1, pentaerythrite 5-7, styrene 115-120, ammonium persulfate 3-4, fire-proof additive 4-
6th, stearic acid 1-2.
A kind of described ester modified fire proofing material of silicic acid, described fire-proof additive are APP, zinc hydroxyl stannate, cunning
One kind in stone flour.
A kind of described ester modified fire proofing material of silicic acid, described esters of silicon acis modified carbon nano-tube is by following weight parts
Raw material composition：
Metasilicic acid 2-3, stearine 0.7-1, maleic anhydride 10-14, trimethyl benzyl ammonia chloride 1-2, diphenyl silicon two
Alcohol 4-5, CNT 10-14, cumyl peroxide 0.2-0.5.
A kind of described ester modified fire proofing material of silicic acid, the preparation method of described esters of silicon acis modified carbon nano-tube include with
Lower step：
（1）CNT is taken, is soaked in the sulfuric acid solution that concentration is 96-98% 2-3 hours, discharging washing, drying, is cooled to
Normal temperature, mixed with maleic anhydride, be added in the dimethylformamide of 1.7-2 times of compound weight, stir, be sent to anti-
Answer in kettle, be passed through nitrogen, regulation temperature of reaction kettle is 65-70 DEG C, adds cumyl peroxide, insulated and stirred 3-4 hours, obtains
Condensing model carbon nano-tube solution；
（2）Trimethyl benzyl ammonia chloride is taken, is added in the deionized water of 20-30 times of its weight, stirs, obtain the aqueous solution；
（3）Stearine, metasilicic acid mixing are taken, is added in the dimethylformamide of 3-4 times of compound weight, in 60-
Insulated and stirred 10-15 minutes at 65 DEG C, obtain acid amides dispersion liquid；
（4）Above-mentioned condensing model carbon nano-tube solution is taken, mixes, stirs with the aqueous solution, rise temperature is 50-60 DEG C, insulation
10-20 minutes are stirred, add diphenyl silanediol, rise temperature is 90-95 DEG C, adds above-mentioned acid amides dispersion liquid, insulated and stirred
2-3 hours, filtering, precipitation is washed, air drying, obtains esters of silicon acis modified carbon nano-tube.
The preparation method of the ester modified fire proofing material of described silicic acid, comprises the following steps：
（1）Fire-proof additive is taken, in ethanol solution that be added to 20-30 times of its weight, 60-65%, adds polydimethylsiloxanes
Alkane, insulated and stirred 1-2 hours, obtain alkyl alcohol solution at 50-60 DEG C；
（2）Pentaerythrite is taken, is heated to 90-95 DEG C, zinc ricinate is added, insulated and stirred 20-30 minutes, is mixed with styrene
Close, be added in abovementioned alkyl alcoholic solution, be sent in reactor, be passed through nitrogen, regulation temperature of reaction kettle is 60-70 DEG C, is added
Enter ammonium persulfate, insulated and stirred 3-5 hours, obtain polystyrene alcoholic solution；
（3）Alkanolamide is taken, is added in the deionized water of 17-20 times of its weight, stirs, adds stearic acid, stirring is equal
It is even, mixed with above-mentioned polystyrene alcoholic solution, rise temperature is 90-95 DEG C, insulated and stirred 1-2 hours, obtains esterification polystyrene
Solution；
（4）Esters of silicon acis modified carbon nano-tube is taken, is added in above-mentioned esterification polystyrene solution, stirs, adds dibutyl
Zinc dithiocarbamate, ultrasonic 10-20 minutes, filtering, precipitation is washed, 3-4 hours, cooling are dried at 50-60 DEG C of vacuum
To normal temperature, the ester modified fire proofing material of the silicic acid is produced.
Advantages of the present invention：
The present invention mixes using maleic anhydride as monomer with CNT, using acid amides as solvent, is polymerize under initiator effect
Reaction, is then added into water and hydrolyzes, esterification is mixed with diphenyl silanediol, and phosphorous ester point is introduced in esterification process
Dispersion liquid, esters of silicon acis modified carbon nano-tube is obtained after drying process；The present invention mixes styrene monomer with pentaerythrite,
Initiator effect is lower to be polymerize, and obtains the polystyrene of containing alcohol, esterification is then mixed with stearic acid, obtain being esterified polystyrene, change
The compatibility being apt between each raw material, improves dispersiveness, effectively reduces reunion, is played to improve the mechanical property of finished product
Good facilitation effect, the esters of silicon acis modified carbon nano-tube that the present invention adds, can in burning by esters of silicon acis modification
To reduce oxygen concentration, good flameproof effect is played, while it is stable carbon-coating that CNT can be formed in burning,
Play good gas phase barriering effect.
Embodiment
Embodiment 1
First, the preparation of esters of silicon acis modified carbon nano-tube
Raw material used is made up of the raw material of following weight parts：
Metasilicic acid 3, stearine 1, maleic anhydride 14, trimethyl benzyl ammonia chloride 2, diphenyl silanediol 5, CNT
14th, cumyl peroxide 0.5.
（1）CNT is taken, is soaked 2 hours in the sulfuric acid solution that concentration is 96%, discharging washing, drying, is cooled to often
Temperature, mixed with maleic anhydride, be added in the dimethylformamide of 2 times of compound weight, stir, be sent to reactor
In, nitrogen is passed through, regulation temperature of reaction kettle is 70 DEG C, adds cumyl peroxide, insulated and stirred 4 hours, obtains condensing model carbon
Nanotube solution；
（2）Trimethyl benzyl ammonia chloride is taken, is added in the deionized water of 30 times of its weight, is stirred, obtain the aqueous solution；
（3）Stearine, metasilicic acid mixing are taken, is added in the dimethylformamide of 4 times of compound weight, at 65 DEG C
Insulated and stirred 15 minutes, obtains acid amides dispersion liquid；
（4）Above-mentioned condensing model carbon nano-tube solution is taken, mixes, stirs with the aqueous solution, rise temperature is 60 DEG C, insulated and stirred
20 minutes, diphenyl silanediol is added, rise temperature is 95 DEG C, adds above-mentioned acid amides dispersion liquid, insulated and stirred 3 hours, filters,
Precipitation is washed, air drying, obtains esters of silicon acis modified carbon nano-tube.
2nd, the preparation of the ester modified fire proofing material of silicic acid
Raw material used is made up of the raw material of following weight parts：
Dimethyl silicone polymer 4, esters of silicon acis modified carbon nano-tube 20, alkanolamide 2, zinc ricinate 1, dibutyl dithio ammonia
Base zinc formate 1, pentaerythrite 7, styrene 120, ammonium persulfate 4, APP 6, stearic acid 2；
Comprise the following steps：
（1）APP is taken, is added in 30 times of its weight, 65% ethanol solution, dimethyl silicone polymer is added, 60
Insulated and stirred 2 hours, obtain alkyl alcohol solution at DEG C；
（2）Pentaerythrite is taken, is heated to 95 DEG C, zinc ricinate is added, insulated and stirred 30 minutes, is mixed with styrene, is added
Into abovementioned alkyl alcoholic solution, it is sent in reactor, is passed through nitrogen, regulation temperature of reaction kettle is 70 DEG C, adds ammonium persulfate,
Insulated and stirred 3-5 hours, obtain polystyrene alcoholic solution；
（3）Alkanolamide is taken, is added in the deionized water of 20 times of its weight, stirs, stearic acid is added, stirs,
Mixed with above-mentioned polystyrene alcoholic solution, rise temperature is 95 DEG C, insulated and stirred 1-2 hours, obtains esterification polystyrene solution；
（4）Esters of silicon acis modified carbon nano-tube is taken, is added in above-mentioned esterification polystyrene solution, stirs, adds dibutyl
Zinc dithiocarbamate, ultrasound 20 minutes, filtering, precipitation is washed, dried 4 hours at 60 DEG C of vacuum, be cooled to normal temperature, i.e.,
Obtain the ester modified fire proofing material of silicic acid.
Embodiment 2
First, the preparation of esters of silicon acis modified carbon nano-tube：
Raw material used is made up of the raw material of following weight parts：
Metasilicic acid 2, stearine 0.7, maleic anhydride 10, trimethyl benzyl ammonia chloride 1, diphenyl silanediol 4, carbon nanometer
Pipe 10, cumyl peroxide 0.2.
（1）CNT is taken, is soaked 3 hours in the sulfuric acid solution that concentration is 96%, discharging washing, drying, is cooled to often
Temperature, mixed with maleic anhydride, be added in the dimethylformamide of 1.7 times of compound weight, stir, be sent to reactor
In, nitrogen is passed through, regulation temperature of reaction kettle is 65 DEG C, adds cumyl peroxide, insulated and stirred 3-4 hours, obtains condensing model
Carbon nano-tube solution；
（2）Trimethyl benzyl ammonia chloride is taken, is added in the deionized water of 20 times of its weight, is stirred, obtain the aqueous solution；
（3）Stearine, metasilicic acid mixing are taken, is added in the dimethylformamide of 3 times of compound weight, at 60 DEG C
Insulated and stirred 10 minutes, obtains acid amides dispersion liquid；
（4）Above-mentioned condensing model carbon nano-tube solution is taken, mixes, stirs with the aqueous solution, rise temperature is 50 DEG C, insulated and stirred
10 minutes, diphenyl silanediol is added, rise temperature is 90 DEG C, adds above-mentioned acid amides dispersion liquid, insulated and stirred 2 hours, filters,
Precipitation is washed, air drying, obtains esters of silicon acis modified carbon nano-tube.
2nd, the preparation of the ester modified fire proofing material of silicic acid
Raw material used is made up of the raw material of following weight parts：
Dimethyl silicone polymer 3, esters of silicon acis modified carbon nano-tube 18, alkanolamide 1, zinc ricinate 0.3, dibutyl dithio
Carbaminate 0.7, pentaerythrite 5, styrene 115, ammonium persulfate 3, zinc hydroxyl stannate 4, stearic acid 1.
（1）Zinc hydroxyl stannate is taken, is added in 20 times of its weight, 60% ethanol solution, adds polydimethylsiloxanes
Alkane, insulated and stirred 1 hour, obtains alkyl alcohol solution at 50 DEG C；
（2）Pentaerythrite is taken, is heated to 90 DEG C, zinc ricinate is added, insulated and stirred 20 minutes, is mixed with styrene, is added
Into abovementioned alkyl alcoholic solution, it is sent in reactor, is passed through nitrogen, regulation temperature of reaction kettle is 60 DEG C, adds ammonium persulfate,
Insulated and stirred 3-5 hours, obtain polystyrene alcoholic solution；
（3）Alkanolamide is taken, is added in the deionized water of 17 times of its weight, stirs, stearic acid is added, stirs,
Mixed with above-mentioned polystyrene alcoholic solution, rise temperature is 90 DEG C, insulated and stirred 1 hour, obtains esterification polystyrene solution；
（4）Esters of silicon acis modified carbon nano-tube is taken, is added in above-mentioned esterification polystyrene solution, stirs, adds dibutyl
Zinc dithiocarbamate, ultrasound 10 minutes, filtering, precipitation is washed, dried 3 hours at 50 DEG C of vacuum, be cooled to normal temperature, i.e.,
Obtain the ester modified fire proofing material of silicic acid.
Performance test：
The ester modified fire proofing material mechanics of silicic acid of the embodiment of the present invention 1, fire resistance test：
Bending strength：775Kg/CM2, the Kg/CM of compressive strength 9112, oxygen index (OI) 29, vertical combustion grade UL-94 V-0 levels；
The ester modified fire proofing material mechanics of silicic acid of the embodiment of the present invention 2, fire resistance test：
Bending strength：801Kg/CM2, the Kg/CM of compressive strength 9432, oxygen index (OI) 29, vertical combustion grade UL-94 V-0 levels；
Commercial polysterol materialogy, fire resistance test：
Bending strength：300-500 Kg/CM2, compressive strength 600-800 Kg/CM2, oxygen index (OI) 27, vertical combustion grade UL-
94 V-1 levels.
As can be seen that the ester modified fire proofing material of silicic acid of the present invention has more preferable mechanical property and fire retardant performance.
Claims (5)
1. a kind of ester modified fire proofing material of silicic acid, it is characterised in that it is made of the raw material of following weight parts：
Dimethyl silicone polymer 3-4, esters of silicon acis modified carbon nano-tube 18-20, alkanolamide 1-2, zinc ricinate 0.3-1, two
Zinc dibutyl dithiocarbamate 0.7-1, pentaerythrite 5-7, styrene 115-120, ammonium persulfate 3-4, fire-proof additive 4-
6th, stearic acid 1-2.
2. the ester modified fire proofing material of a kind of silicic acid according to claim 1, it is characterised in that described fire-proof additive is
One kind in APP, zinc hydroxyl stannate, talcum powder.
A kind of 3. ester modified fire proofing material of silicic acid according to claim 1, it is characterised in that described esters of silicon acis carbon modified
Nanotube is made up of the raw material of following weight parts：
Metasilicic acid 2-3, stearine 0.7-1, maleic anhydride 10-14, trimethyl benzyl ammonia chloride 1-2, diphenyl silicon two
Alcohol 4-5, CNT 10-14, cumyl peroxide 0.2-0.5.
A kind of 4. ester modified fire proofing material of silicic acid according to claim 3, it is characterised in that described esters of silicon acis carbon modified
The preparation method of nanotube comprises the following steps：
（1）Above-mentioned CNT is taken, is soaked in the sulfuric acid solution that concentration is 96-98% 2-3 hours, discharging washing, is dried, it is cold
But to normal temperature, mixed with maleic anhydride, be added in the dimethylformamide of 1.7-2 times of compound weight, stir, be sent into
Into reactor, nitrogen is passed through, regulation temperature of reaction kettle is 65-70 DEG C, adds cumyl peroxide, insulated and stirred 3-4 is small
When, obtain condensing model carbon nano-tube solution；
（2）Trimethyl benzyl ammonia chloride is taken, is added in the deionized water of 20-30 times of its weight, stirs, obtain the aqueous solution；
（3）Stearine, metasilicic acid mixing are taken, is added in the dimethylformamide of 3-4 times of compound weight, in 60-
Insulated and stirred 10-15 minutes at 65 DEG C, obtain acid amides dispersion liquid；
（4）Above-mentioned condensing model carbon nano-tube solution is taken, mixes, stirs with the aqueous solution, rise temperature is 50-60 DEG C, insulation
10-20 minutes are stirred, add diphenyl silanediol, rise temperature is 90-95 DEG C, adds above-mentioned acid amides dispersion liquid, insulated and stirred
2-3 hours, filtering, precipitation is washed, air drying, obtains esters of silicon acis modified carbon nano-tube.
5. the preparation method of the ester modified fire proofing material of a kind of silicic acid as claimed in claim 1, it is characterised in that including following step
Suddenly：
（1）Fire-proof additive is taken, in ethanol solution that be added to 20-30 times of its weight, 60-65%, adds polydimethylsiloxanes
Alkane, insulated and stirred 1-2 hours, obtain alkyl alcohol solution at 50-60 DEG C；
（2）Pentaerythrite is taken, is heated to 90-95 DEG C, zinc ricinate is added, insulated and stirred 20-30 minutes, is mixed with styrene
Close, be added in abovementioned alkyl alcoholic solution, be sent in reactor, be passed through nitrogen, regulation temperature of reaction kettle is 60-70 DEG C, is added
Enter ammonium persulfate, insulated and stirred 3-5 hours, obtain polystyrene alcoholic solution；
（3）Alkanolamide is taken, is added in the deionized water of 17-20 times of its weight, stirs, adds stearic acid, stirring is equal
It is even, mixed with above-mentioned polystyrene alcoholic solution, rise temperature is 90-95 DEG C, insulated and stirred 1-2 hours, obtains esterification polystyrene
Solution；
（4）Esters of silicon acis modified carbon nano-tube is taken, is added in above-mentioned esterification polystyrene solution, stirs, adds dibutyl
Zinc dithiocarbamate, ultrasonic 10-20 minutes, filtering, precipitation is washed, 3-4 hours, cooling are dried at 50-60 DEG C of vacuum
To normal temperature, the ester modified fire proofing material of the silicic acid is produced.
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| CN108912678A (en) * | 2018-05-30 | 2018-11-30 | 查公祥 | A kind of polyanhydride modified polypyrrole conductive additive and preparation method thereof |
| CN109629031A (en) * | 2018-10-29 | 2019-04-16 | 董荣志 | A kind of bisphenol-A doping conductive fiber and preparation method thereof |
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| CN109629031A (en) * | 2018-10-29 | 2019-04-16 | 董荣志 | A kind of bisphenol-A doping conductive fiber and preparation method thereof |
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