CN107603020A - A kind of method that anti-flaming function masterbatch is prepared by gel method - Google Patents
A kind of method that anti-flaming function masterbatch is prepared by gel method Download PDFInfo
- Publication number
- CN107603020A CN107603020A CN201710990424.0A CN201710990424A CN107603020A CN 107603020 A CN107603020 A CN 107603020A CN 201710990424 A CN201710990424 A CN 201710990424A CN 107603020 A CN107603020 A CN 107603020A
- Authority
- CN
- China
- Prior art keywords
- flame retardant
- flaming function
- prepared
- microcapsule
- masterbatch
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Fireproofing Substances (AREA)
Abstract
The invention belongs to flame retardant area, more particularly to a kind of method that anti-flaming function masterbatch is prepared by gel method, it is characterized in that, limitation is by microcapsule phosphorus flame retardant, then aluminum nitrate solution, butyl titanate, ammoniacal liquor are added in high-speed mixer, alumina packing and microcapsule phosphorus flame retardant etc. are added into mixed at high speed again, form gel mixture, microcapsule flame retardant evenly spreads to inside gel and firmly adsorbed, most gained mixed gel is dried, crushed at last, and the anti-flaming function masterbatch is made.The method step is simple, prepares gel quickly and can effectively disperse, and without preparing masterbatch by melting extrusion granulation, equipment cost and energy consumption are low, is adapted to large-scale production.
Description
Technical field
The invention belongs to flame retardant area, and in particular to a kind of method that anti-flaming function masterbatch is prepared by gel method.
Background technology
With the development of science and technology growth in the living standard, high polymer material especially synthesizes macromolecule：Such as plastics, rubber
Status in people live is more and more important, its trend expanded year by year using presenting.But most high-molecular organic material
With inflammable characteristic different degrees of in air, in order to realize it in military, space flight, traffic, electric power and all multirows such as civilian
The application of industry, it is carried out flame-retardant modified to turn into new problem.It is more satisfactory at present to be often to plastic flame method of modifying
Product by adding fire retardant or flame-retardant master batch etc improves the fire protecting performance of plastics.
Fire-retardant master granule, flame-retardant master batch, fire-retardant particle, master batch of preventing fires, fire prevention masterbatch etc. can also be called, be current plastics resistance
Fire in the market and show flame retardant products the most excellent.Popular says, fire-retardant master granule is exactly the concentration mother after fire retardant compound prescription
Grain, by carrier and composite flame-retardant agent, twin-screw is granulated and formed.It is different from fire retardant, its dispersiveness in material resin, flowing
Property, compatibility, heat endurance and weatherability etc. be all far superior to common flame retardant products.Flame-retardant master batch has in resin easily
In addition, sanitation and hygiene, flame retarding efficiency is high, and addition is small, small to the Effect on Mechanical Properties of resin, is not susceptible to after addition point
The bad phenomenons such as layer, decorative pattern, precipitation, human and material resources cost and time are saved, dust is not produced in process, can protect
Workshop condition and the health of worker.In general dispersiveness of the flame-retardant master batch in resin, mobility are compatible with resin
Property and heat endurance and weather resistance be all significantly better than conventional flame retardant, be formulated in addition its flame retarding efficiency of proper flame-retardant master batch and
Efficiency（Cost performance）Also conventional flame retardant is much better than.So flame-retardant master batch realizes fire protection requirement as flame retardant plastic products at present
One of optimal selection, and as effective substitute of fire retardant powder.
The main component of flame-retardant master batch includes fire retardant, heat stabilizer, vector resin and other parts of auxiliary agent four.Fire retardant
Often selection organohalogen compounds-inorganic combustion inhibitor compound system, organohalogen compounds-auxiliary flame retardant antimonial, antismoke agent aluminum oxide
Deng complex, to produce cooperative effect.What main flame retardant organohalogen compounds were commonly used has eight bromo ether, tetrabromobisphenol A, decabrominated dipheny
Ether, HBCD etc., its flame retardant effect are excellent.Inorganic combustion inhibitor mainly has aluminium hydroxide, magnesium hydroxide etc., their costs
It is low, non-secondary pollution, but flame retardant effect is poor.Auxiliary flame retardant is mainly antimony oxide and aluminium dioxide (and antismoke agent) etc..Heat
Dibasicity aluminium phosphite, organic tin, epoxide, superfluous mixture etc. are several for stabilizer conventional mainly having, more from multiple
With thing, to play its cooperative effect.Vector resin mainly has polyolefin and its copolymer, such as LDPE, HDPE, PP, LLDPE etc.
The carrier of Polyolefin Fire-resistant Master Batch can all be made.And phenylethylene flame-retardant master batch vector resin can be selected CPE, EVA., ACR,
SBS.Dispersant it is conventional have Tissuemat E, OPE, polypropylene wax, a- methylstyrene resins, stearic acid and its
Salt, paraffin etc..Compound dispersing agent of the multiselect to Tissuemat E for main component in masterbatch production.The fire-retardant mother of other auxiliary agents
The kind of flame-retardant master batch processed is different with purposes in addition to four kinds of main components more than for material, also to add lubricant sometimes, according to institute
Coupling agent, antioxidant, ultra-violet absorber, antistatic additive etc., to increase the added value of flame-retardant master batch, turn into multifunctional flame-proof mother
Material.
Traditional flame-retardant master batch technology is ripe, but its production process all needs to use high-speed kneading machine and Screw Extrusion
Machine, not only technique is cumbersome, and equipment cost is high, high energy consumption.Such as masterbatch is prepared according to without using the method for extruder
Grain, then production cost greatly reduces.Based on this, it is low to obtain that this patent provides a kind of anti-flaming function masterbatch prepared by gel method
Cost, high performance fire proofing, meet the needs of actual production.
The content of the invention
The technical problems to be solved by the invention are the defects of presence for prior art, propose that one kind is prepared by gel method
The method of anti-flaming function masterbatch.First aluminum nitrate solution, butyl titanate, ammoniacal liquor are added in high-speed mixer, then by aluminum oxide
Filler and microcapsule phosphorus flame retardant etc. add mixed at high speed, form gel mixture, microcapsule flame retardant evenly spreads to solidifying
Adsorb inside glue and firmly, most gained mixed gel is dried, crushed at last, and the anti-flaming function masterbatch is made.
A kind of method that anti-flaming function masterbatch is prepared by gel method, it is characterized in that：Specific step of preparation process is as follows：
（1）The preparation of microcapsule phosphorus flame retardant：Enter in the reactor for having heating function, mechanical agitation and ultrasonator
OK, it is in the case where opening stirring and ultrasonator, phosphorus flame retardant is dispersed in organic solvent, obtain the resistance of phosphorus system
The dispersion liquid of agent is fired, adds silane coupler and acid binding agent, stops mechanical agitation after temperature is 45 DEG C ~ 90 DEG C 2 ~ 4h of reaction
And ultrasound, room temperature is cooled to, is filtered by vacuum and is dried in vacuo, obtains a kind of powdered phosphorus flame retardant microcapsule flame retardant；
（2）The preparation of anti-flaming function masterbatch：Carried out in the reactor for having heating function, mechanical agitation and ultrasonator,
In the case of opening stirring and ultrasonator, aluminum nitrate, butyl titanate are configured to the aqueous solution, is encased in reactor, adds
Heat is slowly dropped into ammoniacal liquor to 60 ~ 90 DEG C；Ammoniacal liquor continues 30 ~ 60min of stirring after adding after, aluminum oxide and step are added（1）System
Standby microcapsule phosphorus flame retardant, continues 10 ~ 30min of high-speed stirred, and 200 ~ 300r/min of speed of agitator finally obtains gel
Mixture, by drying, crush a kind of anti-flaming function masterbatch of acquisition.
The phosphorus flame retardant be selected from ammonium phosphate, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, APP, tricresyl phosphate,
At least one of triphenyl phosphate, trioctyl phosphate, cresyl diphenyl phosphate.
The organic solvent is selected from dichloromethane, toluene, dimethylbenzene, acetone, butanone, formaldehyde, methanol, ethanol, propyl alcohol, fourth
At least one of alcohol, N'N- dimethyl acetamides, N'N- dimethylformamides.
The silane coupler is selected from gamma-aminopropyl-triethoxy-silane（KH550）, γ-(oxygen of 2,3- epoxies third) propyl group
Trimethoxy silane（KH560）, γ-methacryloxypropyl trimethoxy silane（KH570）, γ-the ethoxy of mercapto propyl group three
Base silane（KH580）, γ-mercaptopropyl trimethoxysilane（KH590）At least one of, silane coupler and phosphorus flame retardant
Weight ratio be 1:0.5~1.5.
The acid binding agent is selected from least one of triethylamine, sodium carbonate, pyridine or alkoxy pyridines, acid binding agent and silane
The weight ratio of coupling agent is 1:2~4.
Step（1）The process conditions of the vacuum filtration are leaked to keep vacuum in 0.08Pa ~ 0.10Pa using core
Bucket, uses middling speed type double-layer filter paper；The vacuum drying vacuum is 0.05Pa ~ 0.1Pa, and temperature is 75 ~ 85 DEG C, and vacuum is done
The dry time is 6 ~ 24h.
The aluminum nitrate in terms of aluminium ion, butyl titanate is in terms of titanium ion, ammoniacal liquor in terms of ammonium ion, the mol ratio of three is
1:0.05~0.3:4~6。
The aluminum oxide is conventional commercial alumina powder, and particle diameter is 20 ~ 200 μm；Aluminum oxide and microcapsules phosphorous flame-retardant
Agent is with mass ratio 1:1 adds, and total addition of aluminum oxide and microcapsule phosphorus flame retardant is aluminum nitrate, butyl titanate gross mass
3-5 times.
Step（2）The drying is vacuum drying, and for drying temperature at 140 ~ 200 DEG C, vacuum is 0.05Pa ~ 0.1Pa, when
Between be 6 ~ 24h；The air-flow that is broken for crushes, and granularity is 10 ~ 100 μm after crushing.
A kind of method that anti-flaming function masterbatch is prepared by gel method in the present invention, by aluminum nitrate solution, butyl titanate with
The dispersed formation gel of aluminum oxide, microcapsule flame retardant, is firmly adsorbed inside gel, and most gained mixed gel is carried out at last
Dry, crush, the anti-flaming function masterbatch is made.Without preparing masterbatch by melting extrusion granulation, and it is uniformly dispersed, equipment
Cost and energy consumption are low, are adapted to large-scale production.
It is directly appended to using the application method with reference to general flame-retardant master batch in polymeric matrix, the polymeric matrix can
Think polypropylene, polyethylene, makrolon, polyimides, polyformaldehyde etc..
Compared with prior art, a kind of method that anti-flaming function masterbatch is prepared by gel method in the present invention, what is had is beneficial
Effect is：
1st, a kind of method that anti-flaming function masterbatch is prepared by gel method is proposed, its technical characteristic is, system simple in this method and step
Standby gel is quick and can effectively disperse, and without preparing masterbatch by melting extrusion granulation, equipment cost and energy consumption are low, is adapted to scale
Metaplasia is produced.
2nd, the present invention uses the phosphorus flame retardant of internal capsule-core and polymeric matrix to separate, initial stage not by external influence,
And under suitable condition, cyst wall rupture cause capsule-core directly act on polymeric matrix, to it is controllable fire-retardant and it is different burn into
The fire-retardant control of journey.
3rd, a kind of anti-flaming function masterbatch prepared by gel method in the present invention, capital equipment is all conventional sets in production technology
It is standby, and equipment investment is few, and technique is simple, is easily controlled, and cost is cheap, and preparation process and use process are without poisonous and harmful gas
Body, comply fully with environmental requirement.
Embodiment
Below by way of embodiment, the present invention is described in further detail, but this should not be interpreted as to the present invention
Scope be only limitted to following example.In the case where not departing from above method thought of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
A kind of method that anti-flaming function masterbatch is prepared by gel method, there is the anti-of heating function, mechanical agitation and ultrasonator
Answer in kettle and carry out, first prepare microcapsule phosphorus flame retardant, then prepare anti-flaming function masterbatch：
A, in the case where opening the mechanical agitation of reactor and ultrasonator, trioctyl phosphate is dispersed in toluene
In, KH550 is added, the weight ratio of itself and trioctyl phosphate is 1:0.5, triethylamine is added, itself and KH550 weight ratio are
1:2.Stop mechanical agitation and ultrasound after temperature is 45 DEG C of reaction 2h, be cooled to room temperature, be filtered by vacuum, in 0.05Pa, temperature
For 75 DEG C, 6h is dried in vacuo, obtains a kind of powdered phosphorus flame retardant microcapsule flame retardant.
B, open stirring and ultrasonator in the case of, aluminum nitrate, butyl titanate are configured to the aqueous solution, according to than
Example is encased in reactor, is heated to 60 DEG C, in the case where opening stirring and ultrasonator, is slowly dropped into ammoniacal liquor；Ammoniacal liquor
Continue after adding after stirring 30min, add aluminum oxide and microcapsule phosphorus flame retardant, continue high-speed stirred 10min, stirring turns
Fast 200r/min finally obtains gelatinous mixture, by drying, crushes a kind of anti-flaming function masterbatch of acquisition.The aluminum nitrate with
Aluminium ion meter, butyl titanate is in terms of titanium ion, ammoniacal liquor in terms of ammonium ion, the mol ratio of three is 1:0.05:4；Aluminum oxide with it is micro-
Capsule phosphorus flame retardant is with mass ratio 1:1 adds, and total addition of aluminum oxide and microcapsule phosphorus flame retardant is aluminum nitrate, metatitanic acid
3 times of butyl ester gross mass.The drying is vacuum drying, and drying temperature is at 140 DEG C, vacuum 0.05Pa, time 6h；Institute
State and be broken for air-flow and crush, granularity is 10 μm after crushing.
The flame-retardant master batch that embodiment 1 is obtained is used for polypropylene fire retardant with 5% mass ratio, and fire resistance reaches V-0
Level, shows as excellent flame-retarding characteristic.
By analysis, each particulate is a complete flame-retardant system in flame-retardant master batch prepared by gel method, internal
The phosphorus flame retardant of capsule-core separates with polymeric matrix, and initial stage, cyst wall ruptured not by external influence, and under suitable condition
So that capsule-core directly acts on polymeric matrix, the fire-retardant control of controllable fire-retardant and different flame mechanisms.
Embodiment 2
A kind of preparation of the anti-flaming function masterbatch prepared by gel method is having the anti-of heating function, mechanical agitation and ultrasonator
Answer in kettle and carry out, first prepare microcapsule phosphorus flame retardant, then prepare anti-flaming function masterbatch：
A, in the case where opening the mechanical agitation of reactor and ultrasonator, ammonium phosphate is dispersed in toluene, then
KH560 is added, the weight ratio of itself and ammonium phosphate is 1:0.5, triethylamine is added, itself and KH560 weight ratio are 1:3.In temperature
Spend to stop mechanical agitation and ultrasound after 60 DEG C of reaction 3h, be cooled to room temperature, be filtered by vacuum, in 0.07Pa, temperature is 75 DEG C, very
Sky dries 12h, obtains a kind of powdered phosphorus flame retardant microcapsule flame retardant.
B, open stirring and ultrasonator in the case of, aluminum nitrate, butyl titanate are configured to the aqueous solution, according to than
Example is encased in reactor, is heated to 70 DEG C, in the case where opening stirring and ultrasonator, is slowly dropped into ammoniacal liquor；Ammoniacal liquor
Continue after adding after stirring 30min, add aluminum oxide and the microcapsule phosphorus flame retardant of first step preparation, continue high-speed stirred
10min, speed of agitator 200r/min finally obtain gelatinous mixture, by drying, crush a kind of anti-flaming function masterbatch of acquisition.
The aluminum nitrate in terms of aluminium ion, butyl titanate is in terms of titanium ion, ammoniacal liquor in terms of ammonium ion, the mol ratio of three is 1:0.1:5；
Aluminum oxide is with microcapsule phosphorus flame retardant with mass ratio 1:1 adds, and total addition of aluminum oxide and microcapsule phosphorus flame retardant is
45 times of aluminum nitrate, butyl titanate gross mass.The drying be vacuum drying, drying temperature at 170 DEG C, vacuum 0.1Pa,
Time is 12h；The air-flow that is broken for crushes, and granularity is 50 μm after crushing.
Embodiment 3
A kind of preparation of the anti-flaming function masterbatch prepared by gel method is having the anti-of heating function, mechanical agitation and ultrasonator
Answer in kettle and carry out, first prepare microcapsule phosphorus flame retardant, then prepare anti-flaming function masterbatch：
A, open reactor mechanical agitation and ultrasonator in the case of, by ammonium dihydrogen phosphate be dispersed in toluene,
In dimethylbenzene mixed liquor, KH560 is added, the weight ratio of itself and ammonium dihydrogen phosphate is 1:1.5, alkoxy pyridines are added, its
Weight ratio with KH570 is 1:4.Stop mechanical agitation and ultrasound after temperature is 75 DEG C of reaction 4h, be cooled to room temperature, vacuum is taken out
Filter, in 0.08Pa, temperature is 75 DEG C, is dried in vacuo 24h, obtains a kind of powdered phosphorus flame retardant microcapsule flame retardant.
B, open stirring and ultrasonator in the case of, aluminum nitrate, butyl titanate are configured to the aqueous solution, according to than
Example is encased in reactor, is heated to 80 DEG C, in the case where opening stirring and ultrasonator, is slowly dropped into ammoniacal liquor；Ammoniacal liquor
Continue after adding after stirring 30min, add aluminum oxide and the microcapsule phosphorus flame retardant of first step preparation, continue high-speed stirred
10min, speed of agitator 200r/min finally obtain gelatinous mixture, by drying, crush a kind of anti-flaming function masterbatch of acquisition.
The aluminum nitrate in terms of aluminium ion, butyl titanate is in terms of titanium ion, ammoniacal liquor in terms of ammonium ion, the mol ratio of three is 1:0.2:6；
Aluminum oxide is with microcapsule phosphorus flame retardant with mass ratio 1:1 adds, and total addition of aluminum oxide and microcapsule phosphorus flame retardant is
5 times of aluminum nitrate, butyl titanate gross mass.The drying be vacuum drying, drying temperature at 200 DEG C, vacuum 0.05Pa,
Time is 24h；The air-flow that is broken for crushes, and granularity is 100 μm after crushing.
Embodiment 4
A kind of preparation of the anti-flaming function masterbatch prepared by gel method is having the anti-of heating function, mechanical agitation and ultrasonator
Answer in kettle and carry out, first prepare microcapsule phosphorus flame retardant, then prepare anti-flaming function masterbatch：
A, in the case where opening the mechanical agitation of reactor and ultrasonator, diammonium hydrogen phosphate is dispersed in acetone
In, KH570 is added, the weight ratio of itself and diammonium hydrogen phosphate is 1:1, pyridine is added, itself and KH570 weight ratio are 1:
3.5.Stop mechanical agitation and ultrasound after temperature is 90 DEG C of reaction 3h, be cooled to room temperature, be filtered by vacuum, in 0.1Pa, temperature is
75 DEG C, 12h is dried in vacuo, obtains a kind of powdered phosphorus flame retardant microcapsule flame retardant.
B, open stirring and ultrasonator in the case of, aluminum nitrate, butyl titanate are configured to the aqueous solution, according to than
Example is encased in reactor, is heated to 90 DEG C, and in the case where opening stirring and ultrasonator, it is molten to be slowly dropped into ammonium hydrogen carbonate
Liquid；Ammonium bicarbonate soln continues after adding after stirring 60min, adds aluminum oxide and the microcapsules phosphorous flame-retardant of first step preparation
Agent, continuation high-speed stirred 10,30min, speed of agitator 200r/min finally obtain gelatinous mixture, by drying, crush and obtain
Obtain a kind of anti-flaming function masterbatch.The aluminum nitrate is in terms of aluminium ion, and butyl titanate is in terms of titanium ion, ammonium hydrogen carbonate is with ammonium ion
Meter, the mol ratio of three is 1:0.3:5；Aluminum oxide is with microcapsule phosphorus flame retardant with mass ratio 1:1 adds, aluminum oxide and micro- glue
Total addition of capsule phosphorus flame retardant is aluminum nitrate, 5 times of butyl titanate gross mass.The drying is vacuum drying, dries temperature
Degree is at 160 DEG C, vacuum 0.1Pa, time 18h；The air-flow that is broken for crushes, and granularity is 50 μm after crushing.
Embodiment 5
A kind of preparation of the anti-flaming function masterbatch prepared by gel method is having the anti-of heating function, mechanical agitation and ultrasonator
Answer in kettle and carry out, first prepare microcapsule phosphorus flame retardant, then prepare anti-flaming function masterbatch：
A, in the case where opening the mechanical agitation of reactor and ultrasonator, APP is dispersed in dichloromethane
In alkane, butanol mixed liquid, KH590 is added, the weight ratio of itself and APP is 1:1.2, add triethylamine, its with
KH590 weight ratio is 1:2.5.Stop mechanical agitation and ultrasound after temperature is 75 DEG C of reaction 3.5h, be cooled to room temperature, vacuum
Filter, in 0.08Pa, temperature is 75 DEG C, is dried in vacuo 12h, obtains a kind of powdered phosphorus flame retardant microcapsule flame retardant.
B, open stirring and ultrasonator in the case of, aluminum nitrate, butyl titanate are configured to the aqueous solution, according to than
Example is encased in reactor, is heated to 80 DEG C, in the case where opening stirring and ultrasonator, is slowly dropped into urea liquid；
Urea liquid continues after adding after stirring 60min, adds aluminum oxide and the microcapsule phosphorus flame retardant of first step preparation, continues
High-speed stirred 10min, speed of agitator 300r/min finally obtain gelatinous mixture, are obtained by drying, crushing a kind of fire-retardant
Functional master batch.The aluminum nitrate in terms of aluminium ion, butyl titanate is in terms of titanium ion, urea in terms of ammonium ion, the mol ratio of three
For 1:0.25:5.5；Aluminum oxide is with microcapsule phosphorus flame retardant with mass ratio 1:1 adds, aluminum oxide and microcapsule phosphorus flame retardant
Total addition for aluminum nitrate, 3 times of butyl titanate gross mass.The drying is vacuum drying, and drying temperature is at 170 DEG C, very
Reciprocal of duty cycle is 0.05Pa, time 20h；The air-flow that is broken for crushes, and granularity is 50 μm after crushing.
Claims (9)
1. a kind of method that anti-flaming function masterbatch is prepared by gel method, it is characterized in that：Specific step of preparation process is as follows：
（1）The preparation of microcapsule phosphorus flame retardant：Enter in the reactor for having heating function, mechanical agitation and ultrasonator
OK, it is in the case where opening stirring and ultrasonator, phosphorus flame retardant is dispersed in organic solvent, obtain the resistance of phosphorus system
The dispersion liquid of agent is fired, adds silane coupler and acid binding agent, stops mechanical agitation after temperature is 45 DEG C ~ 90 DEG C 2 ~ 4h of reaction
And ultrasound, room temperature is cooled to, is filtered by vacuum and is dried in vacuo, obtains a kind of powdered phosphorus flame retardant microcapsule flame retardant；
（2）The preparation of anti-flaming function masterbatch：Carried out in the reactor for having heating function, mechanical agitation and ultrasonator,
In the case of opening stirring and ultrasonator, aluminum nitrate, butyl titanate are configured to the aqueous solution, is encased in reactor, adds
Heat is slowly dropped into ammoniacal liquor to 60 ~ 90 DEG C；Ammoniacal liquor continues 30 ~ 60min of stirring after adding after, aluminum oxide and step are added（1）System
Standby microcapsule phosphorus flame retardant, continues 10 ~ 30min of high-speed stirred, and 200 ~ 300r/min of speed of agitator finally obtains gel
Mixture, by drying, crush a kind of anti-flaming function masterbatch of acquisition.
A kind of 2. method that anti-flaming function masterbatch is prepared by gel method according to claim 1, it is characterised in that：The phosphorus system
Fire retardant is selected from ammonium phosphate, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, APP, tricresyl phosphate, triphenyl phosphate, phosphoric acid
At least one of three monooctyl esters, cresyl diphenyl phosphate.
A kind of 3. method that anti-flaming function masterbatch is prepared by gel method according to claim 1, it is characterised in that：Organic solvent
Selected from dichloromethane, toluene, dimethylbenzene, acetone, butanone, formaldehyde, methanol, ethanol, propyl alcohol, butanol, N'N- dimethyl acetamides,
At least one of N'N- dimethylformamides.
A kind of 4. method that anti-flaming function masterbatch is prepared by gel method according to claim 1, it is characterised in that：The silane
Coupling agent is selected from gamma-aminopropyl-triethoxy-silane, γ-(oxygen of 2,3- epoxies third) propyl trimethoxy silicane, γ-methyl-prop
In alkene acryloxypropylethoxysilane trimethoxy silane, gamma-mercaptopropyltriethoxysilane, γ-mercaptopropyl trimethoxysilane at least
The weight ratio of one kind, silane coupler and phosphorus flame retardant is 1:0.5~1.5.
A kind of 5. method that anti-flaming function masterbatch is prepared by gel method according to claim 1, it is characterised in that：It is described to tie up acid
Agent is selected from least one of triethylamine, sodium carbonate, pyridine or alkoxy pyridines, and the weight ratio of acid binding agent and silane coupler is
1:2~4。
A kind of 6. method that anti-flaming function masterbatch is prepared by gel method according to claim 1, it is characterised in that：Step（1）
The process conditions of the vacuum filtration use sand core funnel to keep vacuum in 0.08Pa ~ 0.10Pa, double using middling speed type
Layer filter paper；The vacuum drying vacuum is 0.05Pa ~ 0.1Pa, and temperature is 75 ~ 85 DEG C, the vacuum drying time is 6 ~
24h。
A kind of 7. method that anti-flaming function masterbatch is prepared by gel method according to claim 1, it is characterised in that：The nitric acid
Aluminium in terms of aluminium ion, butyl titanate is in terms of titanium ion, ammoniacal liquor in terms of ammonium ion, the mol ratio of three is 1:0.05~0.3:4~6.
A kind of 8. method that anti-flaming function masterbatch is prepared by gel method according to claim 1, it is characterised in that：The oxidation
Aluminium is conventional commercial alumina powder, and particle diameter is 20 ~ 200 μm；Aluminum oxide is with microcapsule phosphorus flame retardant with mass ratio 1:1 adds
Enter, total addition of aluminum oxide and microcapsule phosphorus flame retardant is aluminum nitrate, 3-5 times of butyl titanate gross mass.
A kind of 9. method that anti-flaming function masterbatch is prepared by gel method according to claim 1, it is characterised in that：Step（2）
The drying is vacuum drying, and for drying temperature at 140 ~ 200 DEG C, vacuum is 0.05Pa ~ 0.1Pa, and the time is 6 ~ 24h；It is described
It is broken for air-flow to crush, granularity is 10 ~ 100 μm after crushing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710990424.0A CN107603020A (en) | 2017-10-23 | 2017-10-23 | A kind of method that anti-flaming function masterbatch is prepared by gel method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710990424.0A CN107603020A (en) | 2017-10-23 | 2017-10-23 | A kind of method that anti-flaming function masterbatch is prepared by gel method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107603020A true CN107603020A (en) | 2018-01-19 |
Family
ID=61078863
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710990424.0A Withdrawn CN107603020A (en) | 2017-10-23 | 2017-10-23 | A kind of method that anti-flaming function masterbatch is prepared by gel method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107603020A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108467574A (en) * | 2018-02-28 | 2018-08-31 | 东莞市基烁实业有限公司 | A kind of transparent flame-retarding master batch and PET film and preparation method |
| CN109593281A (en) * | 2018-11-17 | 2019-04-09 | 山东东信新材料科技股份有限公司 | A kind of EPS fire-retardant master granule and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104327549A (en) * | 2014-10-31 | 2015-02-04 | 西南交通大学 | Silica-alumina hydrogel double-coated modified ammonium polyphosphate and application thereof to inflaming retarding polypropylene |
| CN105585737A (en) * | 2016-03-04 | 2016-05-18 | 广东工业大学 | Phosphate microcapsule flame retardant and preparation method and application thereof |
-
2017
- 2017-10-23 CN CN201710990424.0A patent/CN107603020A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104327549A (en) * | 2014-10-31 | 2015-02-04 | 西南交通大学 | Silica-alumina hydrogel double-coated modified ammonium polyphosphate and application thereof to inflaming retarding polypropylene |
| CN105585737A (en) * | 2016-03-04 | 2016-05-18 | 广东工业大学 | Phosphate microcapsule flame retardant and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| [阿联酋]VIKAS MITTAL等: "《耐热阻燃聚合物纳米复合材料》", 31 May 2015, 国防工业出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108467574A (en) * | 2018-02-28 | 2018-08-31 | 东莞市基烁实业有限公司 | A kind of transparent flame-retarding master batch and PET film and preparation method |
| CN108467574B (en) * | 2018-02-28 | 2020-07-10 | 东莞市基烁实业有限公司 | Transparent flame-retardant master batch, PET (polyethylene terephthalate) film and preparation method |
| CN109593281A (en) * | 2018-11-17 | 2019-04-09 | 山东东信新材料科技股份有限公司 | A kind of EPS fire-retardant master granule and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105932200B (en) | Lithium ion battery composite separation membrane and preparation method thereof and lithium ion battery | |
| CN103059435B (en) | Composite polystyrene heat insulation material and preparation method of heat insulation board | |
| CN102093735B (en) | Wood flour/polypropylene wood-plastic composite material using silane modified ammonium polyphosphate as fire retardant and preparation method thereof | |
| CN104327549B (en) | Alumina silica hydrogel double-coating ammonium polyphosphate modifying and the application in polypropylene flame redardant thereof | |
| CN103289181B (en) | Thermoplastic low-smoke zero-halogen flame-retardant polyolefin tight buffer material for optical fiber and preparation method thereof | |
| CN102219957B (en) | Functional masterbatch of halogen-free intumescent flame retardant, and preparation method thereof | |
| CN104693604A (en) | Halogen-free flame retardant glass-fiber reinforced polypropylene composite material and preparation method thereof | |
| CN104693485A (en) | Halogen-free intumescent compound flame retardant and application thereof in high-density polyethylene | |
| CN107841048B (en) | A kind of polypropene composition of sensitization discoloration and its preparation method and application | |
| CN105419064A (en) | Laminated composite metal hydroxide and multifunctional master batch preparation method thereof | |
| CN107603020A (en) | A kind of method that anti-flaming function masterbatch is prepared by gel method | |
| CN102352057B (en) | Non-halogen composite flame retardant and application thereof in preparation of flame retardant thermoplastic elastomer composite | |
| CN109096637A (en) | High-impact weatherability PVC/ABS/PMMA alloy plastic and its preparation | |
| CN106589656B (en) | A kind of fire-retardant master granule and its flame retardant type PVC wood plastic wall board being prepared | |
| CN104262778A (en) | High-impact-resistance halogen-free flame-retardant polypropylene composite material and preparation method thereof | |
| CN102643463B (en) | Flame-retardant polyolefin/modified phosphate glass hybridization material and preparation method thereof | |
| CN108003600A (en) | A kind of flame retardant automotive inside gadget material and preparation method thereof | |
| CN111704769A (en) | Method for preparing flame-retardant polypropylene by utilizing in-situ coating modified ammonium polyphosphate | |
| CN106189049A (en) | A kind of lead-acid accumulator flame-retardant plastic-housing material | |
| CN109134939B (en) | Piperazine modified lignin/magnesium aluminum hydroxide double-coated red phosphorus flame retardant and application thereof in PP | |
| CN109763356A (en) | A kind of environment-friendly dye and preparation method thereof | |
| CN102002122A (en) | Preparation method of nano hydrotalcite/nano zinc oxide composite modified polyvinyl chloride resin | |
| CN108219183A (en) | A kind of flame-retardant modified microspheres and preparation method thereof | |
| CN104592945A (en) | Flame-retardant organic phase-change material and preparation method thereof | |
| CN103980644B (en) | For the compositional flame-retardant master batch and preparation method thereof of organosilane crosslinked polyethylene insulation material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20180119 |
|
| WW01 | Invention patent application withdrawn after publication |