CN102383210A - Phosphor nitrogen fire retardant dispersion and preparation method thereof - Google Patents
Phosphor nitrogen fire retardant dispersion and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a phosphor nitrogen fire retardant dispersion and a preparation method thereof, and belongs to the field of fine chemical engineering. The invention aims to solve problems of weak stability of a fire retardant dispersion prepared from a fire retardant for viscose fiber of a prior art and difficulty to realize large scale industrial production, and provides a phosphor nitrogen fire retardant dispersion and a preparation method thereof. According to the method of the invention, a certain proportion of wetting agent, high-molecular dispersant, deflocculation dispersant and an antifoaming agent are added into a cylinder scoring for dispersion and stirring, etc., so that the phosphor nitrogen fire retardant dispersion disperses uniformly, has good stability, good compatibility with a viscous liquid and good spinnability, and is an acid resistant and alkali resistant fire retardant dispersion with wide application fields. The phosphor nitrogen fire retardant dispersion is mixed with the viscous liquid and treated with spinning moulding and post-treatment to obtain a fiber, which has a limit oxygen index higher than 30 and good physical machinery performance.
Description
Technical field
The present invention relates to a kind of fire retardant dispersion liquid and preparation method thereof, more particularly, the present invention relates to a kind of phosphorus-nitrogen containing flame retardant dispersion liquid and preparation method thereof, belong to field of fine chemical.
Background technology
Viscose have hygroscopicity excellence, easy dyeing, antistatic, be easy to characteristic such as weaving processing and have purposes widely.Yet; Viscose belongs to flammable fiber, is very easily burnt and initiation fire by its textiles of processing, causes significant damage to people's lives and properties; Thereby limited its extensive use; The raising of the Along with people's level of consumption and the enhancing of awareness of safety require the fire-retardant cry of viscose strong increasingly, strong promotion the fire-retardant research of domestic and international viscose.
Be used to produce the fire retardant that FRC adopts at present and be mainly following several kinds: what employing was spun by Austrian Lenzing company and Japanese Japan is the chlorination phosphonate fire retardant, and this fire retardant does not meet environmental requirement owing to contain halogen, and application is restricted; The Danufi L FRC that the rhone-poulenc TF-80 fiber of France and the PER FRC of the U.S. adopt the Kemiraoy company of organosilane ester fire retardant, Finland to produce with waterglass fire retardant production Visil series composite flame-proof viscose, the not halogen-containing organic phosphorus flame retardant of German Hoechest company's employing; And Switzerland Sandoz company adopts Sandoflam-5060 pyrophosphate based flame retardant to produce FRC with the mode of blend; Though these FRCs are not halogen-containing; But because the effective flame-retardant composition in the fire retardant that is adopted is single; Make that the addition of fire retardant is relatively large; Not only influence the physical property of fiber, and improved production cost.
The domestic fire-retardant fire retardant that adopts to viscose is mainly employing two sulfo-pyrophosphates (DDPS) such as Cheng Bowen; Chen Sheng etc. adopt the alkoxycyclotriphosphderivative fire retardant, and employings such as Tian Li silica gel-potash fire retardant has carried out fire-retardant research to viscose.At present, it is silicon-series five-retardant that the peace that Shandong Hailong Co., Ltd. of viscose manufacturer of domestic maximum produces is spun the employed fire retardant of fire resistance fibre, owing to itself be solution, can directly be configured in the preparation process that solution joins viscose.Other solid kind fire retardant then must be processed the dispersion liquid of fire retardant, could produce FRC smoothly; Simultaneously, because homemade fire retardant particle diameter is big, particle diameter distributes problems such as wide and fire retardant dispersion stability difference, and the selling at exorbitant prices of import fire retardant does not finally all realize large-scale industrial production.
Summary of the invention
It is poor that the present invention is intended to solve the fire retardant dispersion stability that viscose in the prior art processes with fire retardant; Be difficult to realize large-scale industrial problem; A kind of fire retardant dispersion liquid and preparation method thereof is provided, has more precisely provided a kind of preparation method and utilization thereof of dispersion liquid and the phosphorus-nitrogen containing flame retardant dispersion liquid that this is applicable to viscose of phosphorus-nitrogen containing flame retardant.
In order to realize the foregoing invention purpose, its concrete technical scheme is following:
A kind of phosphorus-nitrogen containing flame retardant dispersion liquid is characterized in that, comprises the following component of meter by weight:
Phosphorus-nitrogen containing flame retardant 25-30 part, wetting agent 1-2 part, macromolecule dispersing agent 3-5 part, separate flocculant dispersant 1-2 part, antifoaming agent 0.5-1 part, deionized water 60-70 part;
Described phosphorus-nitrogen containing flame retardant is N, N
'-two (5,5-dimethyl-2-phospha-2-sulfo--1,3-diox-2-yl) ethylenediamine;
Described wetting agent is an alcohols, as: ethanol, propyl alcohol, ethylene glycol, propylene glycol, isopropyl alcohol.
Described macromolecule dispersing agent is pH value 7-8, and active component is at polycarboxylate sodium's dispersant or the ammonium polyacrylate of 43-47%.
The said flocculation dispersant of separating is that molecular weight is the alkane hydroxyl amino amidolysis flocculation dispersant B YK-109 of 4000-6000.
Said antifoaming agent is that silicon is antifoaming agent, as: dimethicone, SXP antifoaming agent, SG antifoaming agent, GXP antifoaming agent, OS antifoaming agent, WH_1 antifoaming agent or PGA antifoaming agent.
A kind of preparation method of phosphorus-nitrogen containing flame retardant dispersion liquid is characterized in that: comprise following processing step:
A, with 60-70 part deionized water, 1-2 part wetting agent adds in the scuffing of cylinder bore under rotating speed is the stirring of 100-150 r/min and mixes;
B, with 3-5 part macromolecule dispersing agent, 1-2 part is separated flocculant and is put into scuffing of cylinder bore, is to carry out high speed dispersion 10-20 min under the 300-400 r/min at rotating speed;
C, speed of agitator is reduced to 150-200 r/min, the antifoaming agent with 0.5-1 part adds in the scuffing of cylinder bore while stirring;
D, treating the bubble cancellation, is under the stirring of 250-350 r/min at rotating speed, and the phosphorus-nitrogen containing flame retardant with 25-30 part slowly adds in the scuffing of cylinder bore dispersed with stirring 20-30 min simultaneously;
E, with gained soln using ball mill grinding 2-3 h, to particle diameter be 100-500nm, promptly obtain a kind of phosphorus-nitrogen containing flame retardant dispersion liquid that is applicable to viscose according to the invention.
A kind of phosphorus-nitrogen containing flame retardant dispersion liquid provided by the invention can be applied in the production of FRC well.
The fire retardant dispersion liquid that the present invention makes has following advantage:
1, in the production process of viscose, viscose enters into coagulating bath regeneration, is shaped through spinning head; Because the aperture of spinning head is merely about 0.6mm; Particle diameter requirement to adding ingredient is very high, need reach below the 500nm, and require dispersion liquid to have good dispersiveness and stable stability; Can not flocculate; Lamination, otherwise can the production of viscose be impacted, will have a strong impact on the physical and mechanical properties and the fire resistance of finished fiber simultaneously.Phosphorus-nitrogen containing flame retardant N among the present invention, N
'-two (5,5-dimethyl-2-phospha-2-sulfo--1,3-diox-2-yl) ethylenediamine is the needle-like white crystal; Contain the fire-retardant composition of phosphorus nitrogen simultaneously, water insoluble, about initial size 30um; Can not directly apply to fire proofing, after disperseing, grinding, its particle diameter has reached application requirements; It is joined in the material, can not influence the mechanical performance of material itself basically, will give material good flame retardant effect simultaneously.Make its particle diameter that grinds the back fire retardant reach the scope of 100-500nm through adding various auxiliary agents, thereby solved above-mentioned problem.
2, conciliate the flocculation dispersant through a certain proportion of wetting agent of adding, macromolecule dispersing agent, the dispersion liquid that makes not only is uniformly dispersed, depositing the difficult deposition in back, layering for a long time, can mix with viscose glue stoste simultaneously and not take place to reunite simultaneously.
3, add suitable antifoaming agent, reduce the bubble in the dispersion liquid, the feasible forming effect that mixes the aeration fiber of back generation with viscose glue stoste, foam in the minimizing last handling process that simultaneously can be strong carries out production smoothly.
4, in scuffing of cylinder bore, carry out dispersion at a high speed, stirring etc.; Reduce the sedimentation problem that sinks to the bottom of fire retardant; Make all fire retardants to guarantee that the particle diameter of the fire retardant in the final dispersion liquid is evenly distributed, reduce the generation of fault in the spinning process through similar basically grinding and dispersion process.
5, the phosphorus-nitrogen containing flame retardant dispersion liquid of the present invention's production is uniformly dispersed, has good stability, and is good with the viscose compatibility, has good spinnability, is a kind of acidproof, alkaline-resisting fire-retardant dispersion liquid, has wider Application Areas; The phosphorus-nitrogen containing flame retardant dispersion liquid that the present invention makes is with after viscose mixes, and through the fiber that spinning moulding and post processing make, its limited oxygen index reaches more than 30, and fiber has good physical and mechanical properties simultaneously.
The specific embodiment
Embodiment 1
A kind of phosphorus-nitrogen containing flame retardant dispersion liquid comprises the following component of meter by weight:
25 parts of phosphorus-nitrogen containing flame retardants, 1 part of wetting agent, 3 parts of macromolecule dispersing agents, separate 1 part of flocculant dispersant, 0.5 part of antifoaming agent, 60 parts of deionized waters;
Described phosphorus-nitrogen containing flame retardant is N, N
'-two (5,5-dimethyl-2-phospha-2-sulfo--1,3-diox-2-yl) ethylenediamine;
Described macromolecule dispersing agent is a pH value 7, and active component is at polycarboxylate sodium's dispersant of 43%;
The said flocculation dispersant of separating is that molecular weight is 4000 alkane hydroxyl amino amidolysis flocculation dispersant B YK-109.
Embodiment 2
A kind of phosphorus-nitrogen containing flame retardant dispersion liquid comprises the following component of meter by weight:
30 parts of phosphorus-nitrogen containing flame retardants, 2 parts of wetting agents, 5 parts of macromolecule dispersing agents, separate 2 parts of flocculant dispersants, 1 part of antifoaming agent, 70 parts of deionized waters;
Described phosphorus-nitrogen containing flame retardant is N, N
'-two (5,5-dimethyl-2-phospha-2-sulfo--1,3-diox-2-yl) ethylenediamine;
Described macromolecule dispersing agent is a pH value 8, and active component is at polycarboxylate sodium's dispersant of 47%;
The said flocculation dispersant of separating is that molecular weight is 6000 alkane hydroxyl amino amidolysis flocculation dispersant B YK-109.
Embodiment 3
A kind of phosphorus-nitrogen containing flame retardant dispersion liquid comprises the following component of meter by weight:
27.5 parts of phosphorus-nitrogen containing flame retardants, 1.5 parts of wetting agents, 4 parts of macromolecule dispersing agents, separate 1.5 parts of flocculant dispersants, 0.75 part of antifoaming agent, 65 parts of deionized waters;
Described phosphorus-nitrogen containing flame retardant is N, N
'-two (5,5-dimethyl-2-phospha-2-sulfo--1,3-diox-2-yl) ethylenediamine;
Described macromolecule dispersing agent is a pH value 7.5, and active component is at 45% ammonium polyacrylate;
The said flocculation dispersant of separating is that molecular weight is 5000 alkane hydroxyl amino amidolysis flocculation dispersant B YK-109.
Embodiment 4
A kind of phosphorus-nitrogen containing flame retardant dispersion liquid comprises the following component of meter by weight:
29 parts of phosphorus-nitrogen containing flame retardants, 1.1 parts of wetting agents, 4.5 parts of macromolecule dispersing agents, separate 1.7 parts of flocculant dispersants, 0.6 part of antifoaming agent, 66 parts of deionized waters;
Described phosphorus-nitrogen containing flame retardant is N, N
'-two (5,5-dimethyl-2-phospha-2-sulfo--1,3-diox-2-yl) ethylenediamine;
Described macromolecule dispersing agent is a pH value 7.9, and active component is at 44% ammonium polyacrylate;
The said flocculation dispersant of separating is that molecular weight is 5500 alkane hydroxyl amino amidolysis flocculation dispersant B YK-109.
Embodiment 5
On the basis of embodiment 1-4, described wetting agent and antifoaming agent have following preferred version:
1, described wetting agent is ethanol, propyl alcohol, ethylene glycol, propylene glycol or isopropyl alcohol.
2, described antifoaming agent is dimethicone, SXP antifoaming agent, SG antifoaming agent, GXP antifoaming agent, OS antifoaming agent, WH_1 antifoaming agent or PGA antifoaming agent.
Embodiment 6
A kind of preparation method of phosphorus-nitrogen containing flame retardant dispersion liquid comprises following processing step:
A, with 60 parts of deionized waters, 1 part of wetting agent adds in the scuffing of cylinder bore and stirs, and under 100 r/min, mixes;
B, with 3 parts of macromolecule dispersing agents, separate flocculant for 1 part and put into scuffing of cylinder bore, be to carry out high speed dispersion 10 min under 300 r/min at rotating speed;
C, speed of agitator is reduced to 150 r/min, while stirring 0.5 part antifoaming agent is added in the scuffing of cylinder bore;
D, treating the bubble cancellation, is under the stirring of 250 r/min at rotating speed, simultaneously 25 parts phosphorus-nitrogen containing flame retardant is slowly added in the scuffing of cylinder bore dispersed with stirring 20 min;
E, with gained soln using ball mill grinding 2h to particle diameter be 100nm, promptly obtain a kind of phosphorus-nitrogen containing flame retardant dispersion liquid that is applicable to viscose according to the invention.
Embodiment 7
A kind of preparation method of phosphorus-nitrogen containing flame retardant dispersion liquid comprises following processing step:
A, with 70 parts of deionized waters, 2 parts of wetting agents add in the scuffings of cylinder bore and stir, and under 150 r/min, mix;
B, with 5 parts of macromolecule dispersing agents, separate flocculant for 2 parts and put into scuffing of cylinder bore, be to carry out high speed dispersion 20 min under 400 r/min at rotating speed;
C, speed of agitator is reduced to 200 r/min, while stirring 1 part antifoaming agent is added in the scuffing of cylinder bore;
D, treating the bubble cancellation, is under the stirring of 350 r/min at rotating speed, simultaneously 30 parts phosphorus-nitrogen containing flame retardant is slowly added in the scuffing of cylinder bore dispersed with stirring 30 min;
E, with gained soln using ball mill grinding 3h to particle diameter be 500nm, promptly obtain a kind of phosphorus-nitrogen containing flame retardant dispersion liquid that is applicable to viscose according to the invention.
Embodiment 8
A kind of preparation method of phosphorus-nitrogen containing flame retardant dispersion liquid comprises following processing step:
A, with 65 parts of deionized waters, 1.5 parts of wetting agents add in the scuffings of cylinder bore and stir, and under 125 r/min, mix;
B, with 4 parts of macromolecule dispersing agents, separate flocculant for 1.5 parts and put into scuffing of cylinder bore, be to carry out high speed dispersion 15 min under 350 r/min at rotating speed;
C, speed of agitator is reduced to 175 r/min, while stirring 0.75 part antifoaming agent is added in the scuffing of cylinder bore;
D, treating the bubble cancellation, is under the stirring of 300 r/min at rotating speed, simultaneously 27.5 parts phosphorus-nitrogen containing flame retardant is slowly added in the scuffing of cylinder bore dispersed with stirring 25 min;
E, with gained soln using ball mill grinding 2.5h to particle diameter be 300nm, promptly obtain a kind of phosphorus-nitrogen containing flame retardant dispersion liquid that is applicable to viscose according to the invention.
Embodiment 9
A kind of preparation method of phosphorus-nitrogen containing flame retardant dispersion liquid comprises following processing step:
A, with 68 parts of deionized waters, 1.1 parts of wetting agents add in the scuffings of cylinder bore and stir, and under 110 r/min, mix;
B, with 4.8 parts of macromolecule dispersing agents, separate flocculant for 1.7 parts and put into scuffing of cylinder bore, be to carry out high speed dispersion 12 min under 370 r/min at rotating speed;
C, speed of agitator is reduced to 180 r/min, while stirring 0.9 part antifoaming agent is added in the scuffing of cylinder bore;
D, treating the bubble cancellation, is under the stirring of 330 r/min at rotating speed, simultaneously 26 parts phosphorus-nitrogen containing flame retardant is slowly added in the scuffing of cylinder bore dispersed with stirring 21 min;
E, with gained soln using ball mill grinding 2.5h to particle diameter be 200nm, promptly obtain a kind of phosphorus-nitrogen containing flame retardant dispersion liquid that is applicable to viscose according to the invention.
Embodiment 10
The application example of phosphorus-nitrogen containing flame retardant dispersion liquid of the present invention in the preparation FRC:
Take by weighing each raw material by following weight portion (hereinafter to be referred as part):
65 parts of deionized waters, 1.5 parts of ethylene glycol, 4.5 parts of polycarboxylate sodium's dispersants, 1.5 parts of HMW alkane hydroxyl amino acid amides, 0.7 part of antifoaming agent, N, N
'26.8 parts of-two (5,5-dimethyl-2-phospha-2-sulfo--1,3-diox-2-yl) ethylenediamine fire retardants
Production technology:
(1) with 65 parts of deionized waters, it is to mix under 120 r/min that 1.5 parts of ethylene glycol adds in the scuffings of cylinder bore at rotating speed;
(2) with 4.5 parts of polycarboxylate sodium's dispersants, HMW alkane hydroxyl amino acid amides dispersant is put into scuffing of cylinder bore for 1.5 parts, is to carry out high speed dispersion 15 min under 350 r/min at rotating speed;
(3) 0.7 part of organopolysiloxane antifoaming agent is added in the scuffing of cylinder bore, treat till the bubble cancellation;
(4) with N, N
'It is to carry out dispersed with stirring 25 min under 300 r/min that 26.8 parts of-two (5,5-dimethyl-2-phospha-2-sulfo--1,3-diox-2-yl) ethylenediamine fire retardants add in the scuffing of cylinder bore at rotating speed;
(5) gained soln using ball mill is ground 2.5 h, to particle diameter be 250 nm, promptly obtain fire retardant dispersion liquid according to the invention.
The fire retardant dispersion particle size of pressing this explained hereafter is at 250 nm; Favorable dispersibility, no flocculation and delamination phenomenon adds dispersion liquid in the viscose by 20% of alpha-cellulose content; The viscose filter value is 165 ml; Viscosity is 32 s, is a kind of rayon spinning liquid with good spinning property, and its spun viscose index is: do fracture strength: 2.15 cN/dtex; Wet breaking strength: 1.03 cN/dtex; Dried elongation at break: 19%; Line density deviation :-1.0%; Whiteness: 73%; Oil content: 2.5%; Regain: 13%; Residual sulphur rate: 8 mg/100 g; Limited oxygen index (LOI) 31.
Embodiment 11
The application example of phosphorus-nitrogen containing flame retardant dispersion liquid of the present invention in the preparation FRC:
Take by weighing each raw material by following weight (unit: part):
60 parts of deionized waters, 2 parts of ethylene glycol, 5 parts of polycarboxylate sodium's dispersants, 2 parts of HMW alkane hydroxyl amino acid amides, 1 part of antifoaming agent, N, 30 parts of N '-two (5,5-dimethyl-2-phospha-2-sulfo--1,3-diox-2-yl) ethylenediamine fire retardants.
Production technology:
1, with 60 parts of deionized waters, it is to mix under 150 r/min that 2 parts of ethylene glycol adds in the scuffings of cylinder bore at rotating speed;
2, with 5 parts of polycarboxylate sodium's dispersants, HMW alkane hydroxyl amino acid amides dispersant is put into scuffing of cylinder bore for 2 parts, is to carry out high speed dispersion 20min under 400 r/min at rotating speed;
3,1 part of organopolysiloxane antifoaming agent is added in the scuffing of cylinder bore, treat till the bubble cancellation;
4, with N, N
'It is to carry out dispersed with stirring 30 min under 350 r/min that 30 parts of-two (5,5-dimethyl-2-phospha-2-sulfo--1,3-diox-2-yl) ethylenediamine fire retardants add in the scuffing of cylinder bore at rotating speed;
5, gained soln using ball mill is ground 3 h, to particle diameter be 200 nm.
The fire retardant dispersion particle size of pressing this explained hereafter is at 200 nm; Favorable dispersibility, no flocculation and delamination phenomenon adds dispersion liquid in the viscose by 18% of alpha-cellulose content; The viscose filter value is 170ml; Viscosity is 30s, is a kind of rayon spinning liquid with good spinning property, and its spun viscose index is: do fracture strength: 2.05cN/dtex; Wet breaking strength: 1.13 cN/dtex; Dried elongation at break: 19.5%; Line density deviation :-2.0%; Whiteness: 75%; Oil content: 2.3%; Regain: 11%; Residual sulphur rate: 10 mg/100 g; Limited oxygen index (LOI) 33.
Embodiment 12
The application example of phosphorus-nitrogen containing flame retardant dispersion liquid of the present invention in the preparation FRC:
Take by weighing each raw material by following weight (unit: part):
70 parts of deionized waters, 1 part of ethylene glycol, 4 parts of polycarboxylate sodium's dispersants, 1 part of HMW alkane hydroxyl amino acid amides, 0.5 part of antifoaming agent, N, N
'23.5 parts of-two (5,5-dimethyl-2-phospha-2-sulfo--1,3-diox-2-yl) ethylenediamine fire retardants.
Production technology:
1, with 70 parts of deionized waters, it is to mix under 100 r/min that 2 parts of ethylene glycol adds in the scuffings of cylinder bore at rotating speed;
2, with 4 parts of polycarboxylate sodium's dispersants, HMW alkane hydroxyl amino acid amides dispersant is put into scuffing of cylinder bore for 1 part, is to carry out high speed dispersion 18 min under 370 r/min at rotating speed;
3,0.5 part of organopolysiloxane antifoaming agent is added in the scuffing of cylinder bore, treat till the bubble cancellation;
4, with N, N
'It is to carry out dispersed with stirring 25 min under 320 r/min that 23.5 parts of-two (5,5-dimethyl-2-phospha-2-sulfo--1,3-diox-2-yl) ethylenediamine fire retardants add in the scuffing of cylinder bore at rotating speed;
5, gained soln using ball mill is ground 2 h, to particle diameter be 300 nm.
The fire retardant dispersion particle size of pressing this explained hereafter is at 300 nm; Favorable dispersibility, no flocculation and delamination phenomenon adds dispersion liquid in the viscose by 22% of alpha-cellulose content; Anti-flaming viscose liquid filter value is 162.5 ml; Viscosity is 36 s, is a kind of rayon spinning liquid with good spinning property, and its spun viscose index is: do fracture strength: 2.10 cN/dtex; Wet breaking strength: 1.10 cN/dtex; Dried elongation at break: 20.5%; Line density deviation :-1.1%; Whiteness: 78%; Oil content: 2.2%; Regain: 12%; Residual sulphur: 7 mg/100 g; Limited oxygen index (LOI) 31.5.
Claims (7)
1. a phosphorus-nitrogen containing flame retardant dispersion liquid is characterized in that, comprises the following component of meter by weight:
Phosphorus-nitrogen containing flame retardant 25-30 part, wetting agent 1-2 part, macromolecule dispersing agent 3-5 part, separate flocculant dispersant 1-2 part, antifoaming agent 0.5-1 part, deionized water 60-70 part;
Described phosphorus-nitrogen containing flame retardant is N, N
'-two (5,5-dimethyl-2-phospha-2-sulfo--1,3-diox-2-yl) ethylenediamine;
Described macromolecule dispersing agent is pH value 7-8, and active component is at polycarboxylate sodium's dispersant or the ammonium polyacrylate of 43-47%;
The said flocculation dispersant of separating is that molecular weight is the alkane hydroxyl amino amidolysis flocculation dispersant B YK-109 of 4000-6000.
2. a kind of phosphorus-nitrogen containing flame retardant dispersion liquid according to claim 1 is characterized in that: described wetting agent is ethanol, propyl alcohol, ethylene glycol, propylene glycol or isopropyl alcohol.
3. a kind of phosphorus-nitrogen containing flame retardant dispersion liquid according to claim 1 is characterized in that: said antifoaming agent is dimethicone, SXP antifoaming agent, SG antifoaming agent, GXP antifoaming agent, OS antifoaming agent, WH_1 antifoaming agent or PGA antifoaming agent.
4. the preparation method of a kind of phosphorus-nitrogen containing flame retardant dispersion liquid according to claim 1 is characterized in that: comprise following processing step:
A, with 60-70 part deionized water, 1-2 part wetting agent adds in the scuffing of cylinder bore and stirs, and mixes;
B, with 3-5 part macromolecule dispersing agent, 1-2 part is separated flocculant and is put into scuffing of cylinder bore, is to carry out high speed dispersion 10-20 min under the 300-400 r/min at rotating speed;
C, speed of agitator is reduced to 150-200 r/min, the antifoaming agent with 0.5-1 part adds in the scuffing of cylinder bore while stirring;
D, treating the bubble cancellation, is under the stirring of 250-350 r/min at rotating speed, and the phosphorus-nitrogen containing flame retardant with 25-30 part slowly adds in the scuffing of cylinder bore dispersed with stirring 20-30 min simultaneously;
E, be 100-500nm, promptly obtain a kind of phosphorus-nitrogen containing flame retardant dispersion liquid that is applicable to viscose according to the invention gained soln using ball mill grinding to particle diameter.
5. the preparation method of a kind of phosphorus-nitrogen containing flame retardant dispersion liquid according to claim 4 is characterized in that: the rotating speed in the stirring described in the steps A is 100-150 r/min.
6. the preparation method of a kind of phosphorus-nitrogen containing flame retardant dispersion liquid according to claim 4 is characterized in that: the milling time with gained soln using ball mill grinding described in the step e is 2-3h.
7. according to the application of the described a kind of phosphorus-nitrogen containing flame retardant dispersion liquid of one of claim 1-3 in the preparation FRC.
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| CN103614795A (en) * | 2013-11-25 | 2014-03-05 | 常熟市金羽纤维制品厂 | Flame-retardant viscose fiber |
| CN103668951A (en) * | 2013-11-29 | 2014-03-26 | 江苏中新资源集团有限公司 | Fabric flame-retardant finishing agent and preparation method thereof |
| CN104861203A (en) * | 2015-06-17 | 2015-08-26 | 中蓝晨光化工研究设计院有限公司 | Water-based suspension fire retardant containing red phosphorus micro-powder and preparation method and application of fire retardant |
| CN106833081A (en) * | 2017-01-16 | 2017-06-13 | 上海鸿苗实业有限公司 | A kind of phosphorous flame-retardant agent dispersing liquid and preparation method thereof |
| CN110284373A (en) * | 2019-07-26 | 2019-09-27 | 北京知淘科技有限责任公司 | A kind of preparation method and waterproof flame-retardant type corrugated board of waterproof flame-retardant type corrugated board |
| CN110306380A (en) * | 2019-07-26 | 2019-10-08 | 北京知淘科技有限责任公司 | A kind of waterproof flame-retardant paint and preparation method thereof for corrugated board |
| CN113248542A (en) * | 2021-05-24 | 2021-08-13 | 中国纺织科学研究院有限公司 | Flame retardant, flame-retardant Lyocell fiber and preparation method thereof |
| CN115094641A (en) * | 2022-08-13 | 2022-09-23 | 山东巨展新材料有限公司 | Stable flame-retardant dispersion liquid and preparation method thereof |
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| CN103614795A (en) * | 2013-11-25 | 2014-03-05 | 常熟市金羽纤维制品厂 | Flame-retardant viscose fiber |
| CN103668951A (en) * | 2013-11-29 | 2014-03-26 | 江苏中新资源集团有限公司 | Fabric flame-retardant finishing agent and preparation method thereof |
| CN104861203A (en) * | 2015-06-17 | 2015-08-26 | 中蓝晨光化工研究设计院有限公司 | Water-based suspension fire retardant containing red phosphorus micro-powder and preparation method and application of fire retardant |
| CN104861203B (en) * | 2015-06-17 | 2017-09-12 | 中蓝晨光化工研究设计院有限公司 | A kind of red phosphorus micro mist waterborne suspension fire retardant and preparation method and application |
| CN106833081A (en) * | 2017-01-16 | 2017-06-13 | 上海鸿苗实业有限公司 | A kind of phosphorous flame-retardant agent dispersing liquid and preparation method thereof |
| CN110284373A (en) * | 2019-07-26 | 2019-09-27 | 北京知淘科技有限责任公司 | A kind of preparation method and waterproof flame-retardant type corrugated board of waterproof flame-retardant type corrugated board |
| CN110306380A (en) * | 2019-07-26 | 2019-10-08 | 北京知淘科技有限责任公司 | A kind of waterproof flame-retardant paint and preparation method thereof for corrugated board |
| CN110306380B (en) * | 2019-07-26 | 2022-03-29 | 北京知淘科技有限责任公司 | Waterproof flame-retardant coating for corrugated board and preparation method thereof |
| CN113248542A (en) * | 2021-05-24 | 2021-08-13 | 中国纺织科学研究院有限公司 | Flame retardant, flame-retardant Lyocell fiber and preparation method thereof |
| CN115094641A (en) * | 2022-08-13 | 2022-09-23 | 山东巨展新材料有限公司 | Stable flame-retardant dispersion liquid and preparation method thereof |
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