CN102604441A - Organic bentonite for composite flame retardants and preparation process thereof - Google Patents
Organic bentonite for composite flame retardants and preparation process thereof Download PDFInfo
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- CN102604441A CN102604441A CN2012100756715A CN201210075671A CN102604441A CN 102604441 A CN102604441 A CN 102604441A CN 2012100756715 A CN2012100756715 A CN 2012100756715A CN 201210075671 A CN201210075671 A CN 201210075671A CN 102604441 A CN102604441 A CN 102604441A
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Abstract
The invention provides a preparation process for an organic bentonite for composite flame retardants, which adopts sodium bentonite as a raw material to be mixed with composite organic cation surfactant. The preparation process is characterized in that: 3 to 4 parts of sodium hexametaphosphate is added into 300 to 500 parts of deionized water, 30 to 50 parts of sodium bentonite is then added, and after high-speed agitation, bentonite suspension solution is produced; 12 to 20 parts of composite organic cation surfactant is added into 120 to 200 parts of solvent, and after high-speed agitation, composite organic cation surface modifier solution is produced; under the state of high-speed agitation, the composite organic cation surface modifier solution is added into the bentonite suspension solution, ammonia is used for regulating the pH of the mixed solution to be 8 to 9, agitation is carried out under thermostatic waterbath of 75 DEG C to 85 DEG C for 2 hours, centrifugal separation is carried out after the temperature is cooled to the room temperature, and after vacuum drying under 80 DEG C to 90 DEG C and grinding, the organic bentonite for the composite flame retardants is prepared. The organic bentonite obtained by the method has good lipophilicity and a good flame-retardant effect, and can be applied in the modification of paint, ink and plastic, and while the dosage of other flame retardants is reduced and the cost is saved, the flame-retardant property and mechanical property of polymer can be enhanced as well.
Description
Technical field
The invention belongs to wilkinite retrofit technical field, be specifically related to a kind of composite flame-retardant agent and use method for preparing organobentonite.
Background technology
Wilkinite be a kind of be the non-metallic minerals of staple with the smectite; The crystalline structure of smectite is 2: 1 type laminate structures of two silicon-oxy tetrahedron folder layer of aluminum oxygen octahedras; Have good swelling property, adsorptivity, cementability, catalytic, thixotropy, suspension, cationic exchange property and bigger character such as inside and outside specific surface area, have the title of " omnipotent " clay.China's bentonite resource reserves are abundant, are only second to the U.S., occupy the second place of the world.Organobentonite is bentonitic deep processed product, owing to have hydrophobic oil-wet behavior, in organic solvent, has good dispersiveness, adds dissolubility and emulsifying property, therefore is widely used in industries such as plastics, paint, printing ink, petroleum drilling, environmental protection.At present, the bentonite compound method mainly contains wet method, dry method, pre-gelled method and mechanical force and chemical surface-modification method, and wherein wet operations is simple, and modified effect is good, uses the widest.
Existing at present report about organobentonite preparation technology; As: 1, the patent No. is " production method of organic bentonite " employing extrusion modification method of 00101420.X, with octadecyl quaternary ammonium salt and solvent, joins in the material then; In the autothermal extrusion machine, extrude; Obtain the machine wilkinite, this method less investment, high, the suitable scale operation of efficient, shortcoming is that organic content is lower in the gained organobentonite; The oleophylic effect is relatively poor, is not suitable for the application aspect polymer modification; 2, the patent No. is that 200710188484.7 " method for preparing secondary intercalation organic bentonite " adopts transition metal salts such as nickelous nitrate, Xiao Suangu to handle sodium bentonite; Form one time the transition metal ion intercalation; Utilize the cetyl trimethyl ammonia bromide to carry out Secondary Organic formation Secondary Organic intercalation then; Advantage is that gained wilkinite organic degree is higher, and shortcoming is a complicated process of preparation, and cost is higher; Be not suitable for scale prodn, and flame retardant effect is not obvious aspect polymer modification; 3, people such as Liu Zhe of Shenyang University of Technology is a properties-correcting agent with SEPIGEL 305 and stearyl dimethyl benzyl ammonium chloride; Synthetic binary organic modified bentonite; The organobentonite oleophilicity that obtains is better; But because properties-correcting agent is all inflammable organism, its flame retardant resistance is compared raising with inorganic bentonite not obvious.
Organobentonite is applied to superpolymer; Can on nanostructure, carry out compound; The mechanical property of enhancing superpolymer and barrier property etc., but better owing to being generally used for bentonite properties-correcting agent combustionproperty, it is not obvious that the bentonite flame retardant resistance is improved; Thereby after organobentonite is used in superpolymer, flame retardant properties can not be improved significantly.To this; The present invention adopts first can be composite as the organophosphorous fire retardant and the quaternary ammonium salt of fire retardant use separately; Obtain the compound preferably organic cation modifier of flame retardant properties; Handle wilkinite with it, can obtain the good organobentonite of flame retardant properties, significantly widened the bentonite Application Areas.
Summary of the invention
The purpose of this invention is to provide a kind ofly can overcome above-mentioned defective, flame retardant properties is good, technology is simple, with short production cycle, bentonite preparation technology that cost is low, its technical scheme is:
With the sodium bentonite is raw material; Mix with compound organic cats product, it is characterized in that: 3～4 parts of Sodium hexametaphosphate 99s are joined in 300～500 parts of deionized waters, add 30～50 parts of sodium bentonites again; Through high-speed stirring, form the wilkinite aaerosol solution; 12～20 parts of compound organic cats products are joined in 120～200 parts of deionized waters,, form compound organic cationic surface modifier solution through high-speed stirring; Under the state of high-speed stirring; Compound positive organic ion surface-treated agent solution is joined in the bentonite suspension; The pH that uses ammoniacal liquor to regulate mixing solutions is 8～9, stirs 2 hours 75～85 ℃ of waters bath with thermostatic control, is cooled to spinning after the room temperature; In 80～90 ℃ of following vacuum-dryings, pulverizing, but promptly make the organobentonite that composite flame-proof strengthens superpolymer.
Described composite flame-retardant agent is used bentonite preparation technology; Compound organic cationic surface properties-correcting agent is a kind of with Cyagard RF-1 is composite forms by in cetyl trimethyl ammonia bromide, the stearyl dimethyl benzyl ammonium chloride, and wherein its structural formula of Cyagard RF-1 is: [(NCCH
2CH
2)
3PCH
2CH
2P (CH
2CH
2CN
3)]
2+2Br itself is exactly the good environment friendly flame retardant of a kind of flame retardant properties, and itself and the composite compound organic cationic surface properties-correcting agent that obtains of quaternary ammonium salt are had flame-retarding characteristic preferably.
The present invention compared with prior art has following advantage:
(5) composite modifier be made up of Cyagard RF-1 and quaternary ammonium salt of the properties-correcting agent that adopts of the present invention has good flame retardancy, and gained bentonite flame retardant properties is good, oleophilicity by force and interlamellar spacing bigger.
(6) this invention is when modified-high polymer is used, and not only had good dispersiveness but also had the function of fire retardant.In the mechanical property that improves superpolymer, can significantly improve the flame retardant properties of material.
(7) the present invention adopts wet-process modified wilkinite, and technology is simple, and is with short production cycle, and modified effect is good, is fit to industrial production, and the gained organobentonite is applicable to the fire-retardant enhancing modified of superpolymer.
Description of drawings
Accompanying drawing is a process flow sheet of the present invention.
Embodiment
3 parts of Sodium hexametaphosphate 99s are joined in 500 parts of deionized waters, add 50 parts of sodium bentonites again, make 2 bentonite suspensions through high-speed stirring; 10 parts of Cyagard RF-1 and 10 parts of cetyl trimethyl ammonia bromides are joined in 200 parts of deionized waters, and high-speed stirring obtains compound organic cationic surface modifier solution; Under the state of high-speed stirring, the composite cation modifier solution is joined in the bentonite suspension; Using the pH of ammoniacal liquor regulator solution is 8, and reaction is 2 hours under 75 ℃ temperature, leaves standstill and is cooled to normal temperature; Be placed on 80 ℃ of following vacuum-dryings with lower sediment is centrifugal, pulverize and promptly obtain organobentonite.
Through test, gained bentonite performance index are following: density 1.78g/cm
3, whiteness 85%, regain 2.7%, interlamellar spacing 2.685nm.
Embodiment 2
Implementation method is same as embodiment 1, and the add-on that changes Sodium hexametaphosphate 99 is 4 parts, and pH is adjusted to 9.
Embodiment 3
3 parts of Sodium hexametaphosphate 99s are joined in 500 parts of deionized waters, add 50 parts of sodium bentonites again, make bentonite suspension through high-speed stirring; 12 parts of Cyagard RF-1 and 8 parts of cetyl trimethyl ammonia bromides are joined in 200 parts of deionized waters, and high-speed stirring obtains composite cation surface-treated agent solution; Under the state of high-speed stirring, the composite cation modifier solution is joined in the bentonite suspension; Using the pH of ammoniacal liquor regulator solution is 8, and reaction is 2 hours under 75 ℃ temperature, leaves standstill and is cooled to normal temperature; Be placed on 80 ℃ of following vacuum-dryings with lower sediment is centrifugal, pulverize and promptly obtain organobentonite.
Through test, gained bentonite performance index are following: density 1.72g/cm
3, whiteness 83%, regain 2.8%, interlamellar spacing 2.425nm.
Embodiment 4
Implementation method is same as embodiment 3, and the add-on that changes Sodium hexametaphosphate 99 is 4 parts, and pH is adjusted to 9.
Embodiment 5
3 parts of Sodium hexametaphosphate 99s are joined in 500 parts of deionized waters, add 50 parts of sodium bentonites again, make bentonite suspension through high-speed stirring; 10 parts of Cyagard RF-1 and 10 parts of stearyl dimethyl benzyl ammonium chlorides are joined in 200 parts of deionized waters, and high-speed stirring obtains composite cation surface-treated agent solution; Under the state of high-speed stirring, the composite cation modifier solution is joined in the bentonite suspension; Using the pH of ammoniacal liquor regulator solution is 8, and reaction is 2 hours under 75 ℃ temperature, leaves standstill and is cooled to normal temperature; Be placed on 80 ℃ of following vacuum-dryings with lower sediment is centrifugal, pulverize and promptly obtain organobentonite.
Through test, gained bentonite performance index are following: density 1.82g/cm
3, whiteness 87%, regain 2.3%, interlamellar spacing 2.536nm.
Embodiment 6
Implementation method is same as embodiment 5, and the add-on that changes Sodium hexametaphosphate 99 is 4 parts, and pH is adjusted to 9.
Embodiment 7
3 parts of Sodium hexametaphosphate 99s are joined in 500 parts of deionized waters, add 50 parts of sodium bentonites again, make 3 bentonite suspensions through high-speed stirring; 12 parts of Cyagard RF-1 and 8 parts of stearyl dimethyl benzyl ammonium chlorides are joined in 200 parts of deionized waters, and high-speed stirring obtains composite cation surface-treated agent solution; Under the state of high-speed stirring, the composite cation modifier solution is joined in the bentonite suspension; Using the pH of ammoniacal liquor regulator solution is 8, and reaction is 2 hours under 75 ℃ temperature, leaves standstill and is cooled to normal temperature; Be placed on 80 ℃ of following vacuum-dryings with lower sediment is centrifugal, pulverize and promptly obtain organobentonite.
Through test, gained bentonite performance index are following: density 1.80g/cm
3, whiteness 87%, regain 2.5%, interlamellar spacing 2.636nm.
Embodiment 8
Implementation method is same as embodiment 7, and the add-on that changes Sodium hexametaphosphate 99 is 4 parts, and pH is adjusted to 9.
Claims (2)
1. a composite flame-retardant agent is with organobentonite and preparation technology; With the sodium bentonite is raw material; Mix with compound organic cats product, it is characterized in that: 3～4 parts of Sodium hexametaphosphate 99s are joined in 300～500 parts of deionized waters, add 30～50 parts of sodium bentonites again; Through high-speed stirring, form the wilkinite aaerosol solution; 12～20 parts of compound organic cats products are joined in 120～200 parts of deionized waters, and high-speed stirring forms composite cation surface-treated agent solution; Under the state of high-speed stirring; Composite cation surface-treated agent solution is joined in the bentonite suspension; The pH that uses ammoniacal liquor to regulate mixing solutions is 8～9, stirs 2 hours 75～85 ℃ of waters bath with thermostatic control, is cooled to spinning after the room temperature; In 80～90 ℃ of following vacuum-dryings, pulverizing, but promptly make the organobentonite that composite flame-proof strengthens superpolymer.
2. composite flame-retardant agent as claimed in claim 1 is used bentonite preparation technology; It is characterized in that: compound organic cationic surface properties-correcting agent is that a kind of and Cyagard RF-1 in cetyl trimethyl ammonia bromide, the stearyl dimethyl benzyl ammonium chloride is composite, and wherein the structural formula of Cyagard RF-1 is: [(NCCH
2CH
2)
3PCH
2CH
2P (CH
2CH
2CN
3)]
2+2Br itself is exactly the good environment friendly flame retardant of a kind of flame retardant properties, and itself and the composite compound organic cationic surface properties-correcting agent that obtains of quaternary ammonium salt are had flame-retarding characteristic preferably.
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| CN2012100756715A CN102604441A (en) | 2012-03-21 | 2012-03-21 | Organic bentonite for composite flame retardants and preparation process thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104403377A (en) * | 2014-11-22 | 2015-03-11 | 安徽省六安恒源机械有限公司 | Modified bentonite with improved mechanical property and preparation method thereof |
| CN112321900A (en) * | 2020-11-23 | 2021-02-05 | 浙江长安仁恒科技股份有限公司 | Bentonite for flame retardant and preparation method thereof |
-
2012
- 2012-03-21 CN CN2012100756715A patent/CN102604441A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104403377A (en) * | 2014-11-22 | 2015-03-11 | 安徽省六安恒源机械有限公司 | Modified bentonite with improved mechanical property and preparation method thereof |
| CN104403377B (en) * | 2014-11-22 | 2016-05-04 | 安徽省六安恒源机械有限公司 | A kind of modified alta-mud that improves mechanical property and preparation method thereof |
| CN112321900A (en) * | 2020-11-23 | 2021-02-05 | 浙江长安仁恒科技股份有限公司 | Bentonite for flame retardant and preparation method thereof |
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Application publication date: 20120725 |