CN105860140A - Preparation method of aluminum hydroxide/zinc stannate microcapsule flame retardant and product of preparation method - Google Patents
Preparation method of aluminum hydroxide/zinc stannate microcapsule flame retardant and product of preparation method Download PDFInfo
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- CN105860140A CN105860140A CN201610260982.7A CN201610260982A CN105860140A CN 105860140 A CN105860140 A CN 105860140A CN 201610260982 A CN201610260982 A CN 201610260982A CN 105860140 A CN105860140 A CN 105860140A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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Abstract
The invention relates to a preparation method of an aluminum hydroxide/zinc stannate microcapsule flame retardant. The preparation method comprises the following steps: 1) preparing aluminum sulfate into a 5-30 wt% aluminum sulfate solution; 2) adding zinc stannate and a dispersing agent into the aluminum sulfate solution, and dispersing by stirring to obtain a mixed solution; 3) regulating the pH value of the mixed solution to 5-9, and stirring to react; and cooling, filtering, washing, and drying to obtain the aluminum hydroxide/zinc stannate microcapsule flame retardant. The invention also relates to an aluminum hydroxide/zinc stannate microcapsule flame retardant prepared by the preparation method. The aluminum hydroxide/zinc stannate microcapsule flame retardant has the advantages of high flame-retardant efficiency, favorable smoke inhibition property, simple technique and low production equipment investment, can easily implement industrialized production, and can solve the problems in the prior art.
Description
Technical field
The present invention relates to the preparation field of fire retardant, be specifically related to a kind of aluminium hydroxide/zinc microcapsule resistance
The preparation method of combustion agent and product.
Background technology
Along with the development of material science, the application of macromolecular material is more and more extensive, but because itself has
Inflammability, the fire caused is more and more frequent.It is primarily now to be modified by interpolation fire retardant,
Improve its fire resistance, but the fire retardant such as halogen system and antimony oxide can discharge toxic gas when burning,
Discharge a large amount of toxic black smoke as in PVC material combustion process, bring huge to the lives and properties of people
Threaten, so each state is all by researching and developing raw smoke during new technique reduction fire, fire is reduced or eliminated.
Inorganic additive flame retardant aluminium hydroxide and magnesium hydroxide, antimony oxide are widely used,
As Chinese invention patent (CN 102993598 A) discloses the system of a kind of flame-proof polyvinyl chloride granula for cable formula
Standby, its inorganic combustion inhibitor used is magnesium hydroxide, aluminium hydroxide, antimony oxide and expansion type flame-retarding
Agent tetramethylolmethane, these goods have fire resistance and the insulating properties of excellence, but its smoke elimination is inefficient,
Although antimony oxide flame retarding efficiency is preferable, but raw smoke is bigger.In order to reduce raw smoke, researcher
Smoke suppressant is used to replace the fire retardant that raw smoke is big to add in macromolecular material, such as publication number CN
The Chinese patent literature of 104403224 A is open a kind of without antimony flame-retardant polyvinyl chloride wire cable material and system thereof
Preparation Method, this technical patent uses inorganic combustion inhibitor Firebrake ZB, magnesium hydroxide, aluminium hydroxide composite anti-flaming
Polrvinyl chloride, with reduce because of the big problem of raw smoke existed containing antimony, it is possible to reduce pollute, raising environmental protection,
Security performance, but the flame retarding efficiency of this inorganic composite flame retardants is relatively low, when nonflammable material requirement to be met,
Its addition is big, causes material mechanical performance is greatly lowered.
In order to meet highly effective flame-retardant and smoke suppressing simultaneously, researcher be prepared for fire-retardant, press down cigarette synergist,
It mostly is the multielement cooperative flame retardant immunomodulator compounds such as silicon, nitrogen, phosphorus, halogen, such as publication number CN 104744504 A
Chinese patent literature a kind of silicon, nitrogen, the preparation method of halogen multielement cooperative flame retardant immunomodulator compounds are disclosed,
Triglycidyl isocyanurate is used to synthesize in organic solvent with dimethyl two halosilanes, dihalo-propanol
Isocyanuric acid three (dimethyl dihalo-propoxyl group silicon acyloxy halogen propyl group) ester, this type of fire retardant efficiency
Height, smoke effect are good, are suitable as the resistances such as polrvinyl chloride, polyurethane, epoxy resin, unsaturated-resin
Combustion plasticizer, but due to operation is complicated, use organic solvent cause that waste liquid is toxic, plasticizing efficiency relatively
Low, and during materials'use, there is precipitation in various degree in plasticizer, fire retardant durability is poor.
At present, fire retardant and smoke suppressant start to be widely used, but owing to smoke suppressant addition is big, produce
Cost is high, and durability is poor, and is easily caused material mechanical performance and is greatly reduced so that it is materials application field
Limited.
Summary of the invention
Present invention aims to the deficiencies in the prior art, it is provided that a kind of micro-glue of aluminium hydroxide/zinc
The preparation method of capsule fire retardant and product, its flame retarding efficiency is high, and smoke-suppressing is preferable, and technique is simple, produces
Equipment investment is few, and is prone to industrialization production, it is possible to resolve the difficult point of prior art.
Technical scheme provided by the present invention is:
The preparation method of a kind of aluminium hydroxide/zinc microcapsule flame retardant, comprises the steps:
1) it is 5～30% aluminum sulfate solution that aluminum sulfate is configured to mass fraction；
2) zinc and dispersant are joined dispersed with stirring in aluminum sulfate solution, obtain mixed liquor；
3) pH value of regulation mixed liquor is 5～9, stirring reaction；Then filter, wash, dried,
Obtain aluminium hydroxide/zinc microcapsule flame retardant.
Technique scheme provides a kind of technique simple, small investment of production equipment, and it is prone to industrialization
The preparation method of the aluminium hydroxide/zinc microcapsule flame retardant produced, as in figure 2 it is shown, wherein zinc
As the core material of microcapsule, in step 2) in zinc and aluminum sulfate at the effect of dispersant, aluminum sulfate bag
Being rolled in the surface of zinc, then regulation pH value is 5～9, and aluminium hydroxide is slowly on the surface of zinc
Formed, ultimately form aluminium hydroxide/zinc microcapsule.Aluminium hydroxide is as a kind of Halogen, antiacid nothing
Machine fire retardant, with several functions such as filling, fire-retardant, smoke eliminations, and also low price, nontoxic, no
Volatilization, can suppress to burn in the advantage such as generation of molten drop.Zinc as anti-flaming smoke-inhibiting agent, have nontoxic,
Fire-retardant, press down the advantage of cigarette, meet the requirement of current Green Flammability agent, so to its research and development very
Rapidly, the succedaneum of antimony oxide can be become.Due to the decomposition temperature 600 DEG C of zinc, so it can
To be used in polrvinyl chloride, polyester, epoxy resin, nylon etc..Aluminium hydroxide and zinc are to polymeric material
Material has the cooperative flame retardant effect of highly significant, and aluminium hydroxide/zinc microcapsule is possible not only to broader
In temperature range, the liter gentleness of suppression polymer is decomposed, and in succession can release in broader temperature range
Discharge water the concentration of vapor dilution oxygen and fuel gas, and char forming ability is greatly enhanced, and improves cohesion further
Mutually fire-retardant effect, therefore fire resistance increases substantially.
Described aluminum sulfate can be by commercially available acquisition, and aluminum sulfate is preferably aluminum sulfate octadecahydrate, 16 water sulfur
Acid aluminum or 27 water aluminum sulfate.
Described zinc can be by commercially available acquisition.
Described step 3) in the pH value of regulation mixed liquor be 5～9, preferably use weak base aqueous solution class
(such as sodium carbonate or sodium hydroxide solution) can be by commercially available acquisition, and its solution concentration is 5～50%.
As preferably, described step 3) in the pH value of regulation mixed liquor be 5.5～7.5.
As preferably, described aluminum sulfate is 2/8～9/1 with the mass ratio of zinc.Along with cladding shell material hydrogen
The percentage composition of aluminium oxide increases, and aluminium hydroxide/zinc microcapsule flame retardant grain diameter increases, but shell
Material content is unsuitable too high, and otherwise zinc content is too low, affects flame retarding efficiency.
As preferably, described dispersant is sodium hexameta phosphate or sodium lauryl sulphate.Adding of dispersant
Whether adding covered effect impact relatively big, dispersant makes core material be uniformly dispersed in the solution, and covered effect is relatively
Good, and even particle size distribution.
Further preferably, described dispersant is sodium lauryl sulphate/OP-10.OP-10 be emulsifying agent with
Sodium lauryl sulphate compounds, and allows core material disperse in emulsion evenly, it is to avoid a large amount of reunion occurs, makes
Aluminium hydroxide/zinc microcapsule flame retardant even particle size distribution, covered effect is more preferable.
Further preferably, in described dispersant, sodium lauryl sulphate with the mass ratio of OP-10 is
2/1～9/1.Sodium lauryl sulphate and OP-10 mass are than optimum proportioning 3:1, and dispersant is too high, goes out
Existing partial agglomeration phenomenon, reduces the stability of aluminium hydroxide/zinc microcapsule flame retardant.
As preferably, the quality of described dispersant is the 0.1～10% of zinc quality.Its content is most preferably
The 0.5% of zinc, then there is partial agglomeration phenomenon in too high levels, reduces aluminium hydroxide/zinc microcapsule
The stability of fire retardant.
As preferably, described step 2) in the temperature of dispersed with stirring be 30～70 DEG C.
As preferably, described step 3) in the temperature of stirring reaction be 40～70 DEG C, the response time is
2～8h.Reaction temperature is little on the covered effect impact of aluminium hydroxide cladding zinc, and 55 DEG C are more suitable,
Too low then surface is the most coarse, the too high energy consumption that not only increases, and increases cost, and there will be agglomeration,
Affect covered effect.Optimum reacting time is 3h, and the time is the shortest, is coated with uneven, and surface of microcapsule is thick
Rough, and phenomenon of phase separation occurs；Time is oversize, then microcapsule granule agglomeration, impact cladding occur
Effect.
, described step 1 preferred as one) in aluminum sulfate is configured to mass fraction is 8～12% sulphuric acid
Aluminum solutions；Described aluminum sulfate and zinc mass ratio 1～2；Described step 2) in the quality of dispersant
It is the 0.4～0.6% of zinc quality；Described step 3) regulation mixed liquor pH value be 6～7, stirring
Speed 280～320r/min, temperature 50～60 DEG C, the response time 2.8～3.2h.
The present invention also provides for the aluminium hydroxide/zinc microcapsule flame retardant of any of the above-described preparation method gained,
The core material of described aluminium hydroxide/zinc microcapsule flame retardant be zinc, shell material be aluminium hydroxide.When
During the mass ratio 2/3 of aluminium hydroxide/zinc microcapsule, its flame retarding and smoke suppressing properties reaches optimal, Ke Yi great
Amplitude reduces the consumption of fire retardant.The aluminium hydroxide of the present invention/zinc microcapsule flame retardant is white inorganic
Powder is good with the suitability of pigment.It is suitable as polrvinyl chloride, polypropylene, polyethylene, asphalt mixtures modified by epoxy resin
The highly effective flame-retardant smoke suppressant of fat, unsaturated-resin etc..
Compared with the existing technology, beneficial effects of the present invention is embodied in:
(1) aluminium hydroxide of the present invention/zinc microcapsule flame retardant contains the multiple elements such as aluminum, stannum, zinc,
Its cooperative flame retardant efficiency is high, and aluminium hydroxide has fire-retardant and presses down cigarette effect, zinc have highly effective flame-retardant and
Press down cigarette effect, can effectively prevent the generation of molten drop.
(2) aluminium hydroxide of the present invention/zinc microcapsule flame retardant is nucleocapsid structure, and its structural stability is good,
Being more easy to during burning generate fine and close layer of charcoal, smoke effect is excellent.
(3) without adding catalyst etc. in aluminium hydroxide of the present invention/zinc microcapsule flame retardant preparation, no
Introducing impurity element, the equipment that produces is simplified, and process equipment is simple, is suitable for industrialization and produces.
(4) aluminium hydroxide of the present invention/zinc microcapsule flame retardant, zinc price is higher, uses chemistry
Method is prepared as nucleocapsid structure, advantageously reduces this based flame retardant cost, and it is white inorganic powder,
Good with the Adapter Property of pigment, application is extensive.
Accompanying drawing explanation
Fig. 1 is the flow chart preparing aluminium hydroxide/zinc microcapsule flame retardant；
Fig. 2 is the formation figure of aluminium hydroxide/zinc microcapsule flame retardant；
Fig. 3 is transmission electron microscope pattern (a zinc of fire retardant；B aluminium hydroxide/zinc microcapsule).
Detailed description of the invention
Below by embodiment, the present invention is specifically described, it is necessary to it is pointed out here that be following reality
Execute example to be served only for the present invention is further described, it is impossible to be interpreted as limiting the scope of the invention,
Some nonessential improvement and tune that this art skilled person can make according to the content of the invention described above
Whole, still fall within protection scope of the present invention.
Embodiment 1
Preparation flow is as it is shown in figure 1, mechanism as in figure 2 it is shown, be first configured to mass fraction and be by aluminum sulfate
10% aluminum sulfate solution；Then by zinc (aluminum sulfate and zinc mass ratio 1/4) and sodium hexameta phosphate
Dispersant (being the 0.5% of zinc quality) joins dispersed with stirring in aluminum sulfate solution, obtains mixed liquor；
The pH value regulating mixed liquor again is 6.5, mixing speed 300r/min, temperature 55 DEG C, response time 3h；
Finally cool down, filter, wash, dried, obtain aluminium hydroxide/zinc microcapsule flame retardant.
Gained sample carries out TEM morphology characterization, as shown in Figure 3.
Embodiment 2
It is 10% aluminum sulfate solution that aluminum sulfate is first configured to mass fraction；Then by zinc (aluminum sulfate
With zinc mass ratio 1/2) and sodium hexameta phosphate dispersant (being the 0.5% of zinc quality) join sulphuric acid
Dispersed with stirring in aluminum solutions, obtains mixed liquor；The pH value regulating mixed liquor again is 6.5, mixing speed
300r/min, temperature 55 DEG C, response time 3h；Finally cool down, filter, wash, dried,
To aluminium hydroxide/zinc microcapsule flame retardant.
Embodiment 3
It is 10% aluminum sulfate solution that aluminum sulfate is first configured to mass fraction；Then by zinc (aluminum sulfate
With zinc mass ratio 1/1) and sodium hexameta phosphate dispersant (being the 0.5% of zinc quality) join sulphuric acid
Dispersed with stirring in aluminum solutions, obtains mixed liquor；The pH value regulating mixed liquor again is 6.5, mixing speed
300r/min, temperature 55 DEG C, response time 3h；Finally cool down, filter, wash, dried,
To aluminium hydroxide/zinc microcapsule flame retardant.
Embodiment 4
It is 10% aluminum sulfate solution that aluminum sulfate is first configured to mass fraction；Then by zinc (aluminum sulfate
With zinc mass ratio 3/2) and sodium hexameta phosphate dispersant (being the 0.5% of zinc quality) join sulphuric acid
Dispersed with stirring in aluminum solutions, obtains mixed liquor；The pH value regulating mixed liquor again is 6.5, mixing speed
300r/min, temperature 55 DEG C, response time 3h；Finally cool down, filter, wash, dried,
To aluminium hydroxide/zinc microcapsule flame retardant.
Embodiment 5
It is 10% aluminum sulfate solution that aluminum sulfate is first configured to mass fraction；Then by zinc (aluminum sulfate
With zinc mass ratio 2/1) and sodium hexameta phosphate dispersant (being the 0.5% of zinc quality) join sulphuric acid
Dispersed with stirring in aluminum solutions, obtains mixed liquor；The pH value regulating mixed liquor again is 6.5, mixing speed
300r/min, temperature 55 DEG C, response time 3h；Finally cool down, filter, wash, dried,
To aluminium hydroxide/zinc microcapsule flame retardant.
Embodiment 6
It is 10% aluminum sulfate solution that aluminum sulfate is first configured to mass fraction；Then by zinc (aluminum sulfate
With zinc mass ratio 3/1) and sodium hexameta phosphate dispersant (being the 0.5% of zinc quality) join sulphuric acid
Dispersed with stirring in aluminum solutions, obtains mixed liquor；The pH value regulating mixed liquor again is 6.5, mixing speed
300r/min, temperature 55 DEG C, response time 3h；Finally cool down, filter, wash, dried,
To aluminium hydroxide/zinc microcapsule flame retardant.
Embodiment 7
It is 10% aluminum sulfate solution that aluminum sulfate is first configured to mass fraction；Then by zinc (aluminum sulfate
With zinc mass ratio 5/1) and sodium hexameta phosphate dispersant (being the 0.5% of zinc quality) join sulphuric acid
Dispersed with stirring in aluminum solutions, obtains mixed liquor；The pH value regulating mixed liquor again is 6.5, mixing speed
300r/min, temperature 55 DEG C, response time 3h；Finally cool down, filter, wash, dried,
To aluminium hydroxide/zinc microcapsule flame retardant.
Embodiment 8
It is 10% aluminum sulfate solution that aluminum sulfate is first configured to mass fraction；Then by zinc (aluminum sulfate
With zinc mass ratio 1/4) and sodium hexameta phosphate dispersant (being the 0.5% of zinc quality) join sulphuric acid
Dispersed with stirring in aluminum solutions, obtains mixed liquor；The pH value regulating mixed liquor again is 5.5, mixing speed
300r/min, temperature 55 DEG C, response time 3h；Finally cool down, filter, wash, dried,
To aluminium hydroxide/zinc microcapsule flame retardant.
Embodiment 9
It is 10% aluminum sulfate solution that aluminum sulfate is first configured to mass fraction；Then by zinc (aluminum sulfate
With zinc mass ratio 1/4) and sodium hexameta phosphate dispersant (being the 0.5% of zinc quality) join sulphuric acid
Dispersed with stirring in aluminum solutions, obtains mixed liquor；The pH value regulating mixed liquor again is 7.5, mixing speed
300r/min, temperature 55 DEG C, response time 3h；Finally cool down, filter, wash, dried,
To aluminium hydroxide/zinc microcapsule flame retardant.
Embodiment 10
It is 10% aluminum sulfate solution that aluminum sulfate is first configured to mass fraction；Then by zinc (aluminum sulfate
With zinc mass ratio 1/4) and sodium hexameta phosphate dispersant (being the 0.5% of zinc quality) join sulphuric acid
Dispersed with stirring in aluminum solutions, obtains mixed liquor；The pH value regulating mixed liquor again is 9.0, mixing speed
300r/min, temperature 55 DEG C, response time 3h；Finally cool down, filter, wash, dried,
To aluminium hydroxide/zinc microcapsule flame retardant.
Embodiment 11
It is 10% aluminum sulfate solution that aluminum sulfate is first configured to mass fraction；Then by zinc (aluminum sulfate
With zinc mass ratio 1/4) and sodium hexameta phosphate dispersant (being the 0.35% of zinc quality) join sulfur
Dispersed with stirring in acid aluminum solutions, obtains mixed liquor；The pH value regulating mixed liquor again is 6.5, mixing speed
300r/min, temperature 55 DEG C, response time 3h；Finally cool down, filter, wash, dried,
To aluminium hydroxide/zinc microcapsule flame retardant.
Embodiment 12
It is 10% aluminum sulfate solution that aluminum sulfate is first configured to mass fraction；Then by zinc (aluminum sulfate
With zinc mass ratio 1/4) and sodium lauryl sulphate dispersant (being the 0.5% of zinc quality) join
Dispersed with stirring in aluminum sulfate solution, obtains mixed liquor；The pH value regulating mixed liquor again is 6.5, stirring speed
Degree 300r/min, temperature 55 DEG C, response time 3h；Finally cool down, filter, wash, dried,
Obtain aluminium hydroxide/zinc microcapsule flame retardant.
Embodiment 13
It is 10% aluminum sulfate solution that aluminum sulfate is first configured to mass fraction；Then by zinc (aluminum sulfate
With zinc mass ratio 1/4) and OP-10 dispersant (being the 0.5% of zinc quality) to join aluminum sulfate molten
Dispersed with stirring in liquid, obtains mixed liquor；The pH value regulating mixed liquor again is 6.5, mixing speed 300r/min,
Temperature 55 DEG C, response time 3h；Finally cool down, filter, wash, dried, obtain aluminium hydroxide
/ zinc microcapsule flame retardant.
Embodiment 14
It is 10% aluminum sulfate solution that aluminum sulfate is first configured to mass fraction；Then by zinc (aluminum sulfate
With zinc mass ratio 1/4) and 3/1 sodium lauryl sulphate/OP-10 composite dispersing agent (total amount is zinc
The 0.35% of quality) join dispersed with stirring in aluminum sulfate solution, obtain mixed liquor；Regulate mixed liquor again
PH value is 6.5, mixing speed 300r/min, temperature 55 DEG C, response time 3h；Finally cool down, filter,
Washing, dried, obtain aluminium hydroxide/zinc microcapsule flame retardant.
Embodiment 15
It is 10% aluminum sulfate solution that aluminum sulfate is first configured to mass fraction；Then by zinc (aluminum sulfate
With zinc mass ratio 1/4) and 3/1 sodium lauryl sulphate/OP-10 composite dispersing agent (total amount is zinc
The 0.5% of quality) join dispersed with stirring in aluminum sulfate solution, obtain mixed liquor；Regulate mixed liquor again
PH value is 6.5, mixing speed 300r/min, temperature 55 DEG C, response time 3h；Finally cool down, filter,
Washing, dried, obtain aluminium hydroxide/zinc microcapsule flame retardant.
Embodiment 16
It is 10% aluminum sulfate solution that aluminum sulfate is first configured to mass fraction；Then by zinc (aluminum sulfate
With zinc mass ratio 1/4) and sodium hexameta phosphate dispersant (being the 0.5% of zinc quality) join sulphuric acid
Dispersed with stirring in aluminum solutions, obtains mixed liquor；The pH value regulating mixed liquor again is 6.5, mixing speed
300r/min, temperature 25 DEG C, response time 3h；Finally cool down, filter, wash, dried,
To aluminium hydroxide/zinc microcapsule flame retardant.
Embodiment 17
It is 10% aluminum sulfate solution that aluminum sulfate is first configured to mass fraction；Then by zinc (aluminum sulfate
With zinc mass ratio 1/4) and sodium hexameta phosphate dispersant (being the 0.5% of zinc quality) join sulphuric acid
Dispersed with stirring in aluminum solutions, obtains mixed liquor；The pH value regulating mixed liquor again is 6.5, mixing speed
300r/min, temperature 85 DEG C, response time 3h；Finally cool down, filter, wash, dried,
To aluminium hydroxide/zinc microcapsule flame retardant.
Embodiment 18
It is 10% aluminum sulfate solution that aluminum sulfate is first configured to mass fraction；Then by zinc (aluminum sulfate
With zinc mass ratio 1/4) and sodium hexameta phosphate dispersant (being the 0.5% of zinc quality) join sulphuric acid
Dispersed with stirring in aluminum solutions, obtains mixed liquor；The pH value regulating mixed liquor again is 6.5, mixing speed
300r/min, temperature 55 DEG C, response time 1h；Finally cool down, filter, wash, dried,
To aluminium hydroxide/zinc microcapsule flame retardant.
Embodiment 19
It is 10% aluminum sulfate solution that aluminum sulfate is first configured to mass fraction；Then by zinc (aluminum sulfate
With zinc mass ratio 1/4) and sodium hexameta phosphate dispersant (being the 0.5% of zinc quality) join sulphuric acid
Dispersed with stirring in aluminum solutions, obtains mixed liquor；The pH value regulating mixed liquor again is 6.5, mixing speed
300r/min, temperature 55 DEG C, response time 5h；Finally cool down, filter, wash, dried,
To aluminium hydroxide/zinc microcapsule flame retardant.
Embodiment 20
It is 5% aluminum sulfate solution that aluminum sulfate is first configured to mass fraction；Then by zinc (aluminum sulfate with
Zinc mass ratio 1/4) and sodium hexameta phosphate dispersant (being the 0.5% of zinc quality) join aluminum sulfate
Dispersed with stirring in solution, obtains mixed liquor；The pH value regulating mixed liquor again is 6.5, mixing speed
300r/min, temperature 55 DEG C, response time 3h；Finally cool down, filter, wash, dried,
To aluminium hydroxide/zinc microcapsule flame retardant.
Embodiment 21
It is 20% aluminum sulfate solution that aluminum sulfate is first configured to mass fraction；Then by zinc (aluminum sulfate
With zinc mass ratio 1/4) and sodium hexameta phosphate dispersant (being the 0.5% of zinc quality) join sulphuric acid
Dispersed with stirring in aluminum solutions, obtains mixed liquor；The pH value regulating mixed liquor again is 6.5, mixing speed
300r/min, temperature 55 DEG C, response time 3h；Finally cool down, filter, wash, dried,
To aluminium hydroxide/zinc microcapsule flame retardant.
Particle diameter and dispersive property
The preparation process condition of aluminium hydroxide of the present invention/zinc microcapsule flame retardant is different, its particle diameter and grain
Footpath distribution and dispersive property appearance difference in various degree, the most as shown in table 1, in table 1 " uniform,
More uniform, coarse, uneven, poor, preferable, reunite and general " these concepts be embodiment it
Between compare the relative concept obtained.
The different particle diameter of embodiment product of table 1, particle diameter distribution and dispersive property
Fire resistance and smoke suppressing
The nucleocapsid proportioning of aluminium hydroxide of the present invention/zinc microcapsule flame retardant is different, its fire-retardant and smoke-suppressing
Difference in various degree can occur.
Therefore, this programme inventor uses the aluminium hydroxide/zinc microcapsule flame retardant of above-mentioned preparation (in fact
Execute example 2), aluminium hydroxide/zinc microcapsule flame retardant (embodiment 4), the micro-glue of aluminium hydroxide/zinc
As a example by capsule fire retardant (embodiment 6), it is applied in polrvinyl chloride (PVC) film material.
Reference: GB/T 2406.2-2009 " plastics oxygen index method mensuration burning behavior part 2: greenhouse
Test " in the method that provides of non-supported material (thin film) carry out；" construction material fires GB/T 8627-2007
The smoke density test method burnt or decompose " method that provides carries out；FZ/T 64014-2009 " use by membrane structure
Coated fabric the 5.13rd part: the mensuration of combustibility " Plays (GB/T 8626) and (GB/T 20284)
The method provided is carried out；The method that U.S.'s fire proofing rank testing standard ANSI/UL94-1985 provides is entered
OK.
Take respectively above-mentioned fire retardant, plasticizer phthalic acid dinonyl (DINP), barium zinc stabilizer and
After PVC paste resin mix homogeneously in varing proportions, roll with vulcanizing press, make thickness 0.5mm
Sample, test its fire resistance and smoke suppressing, part test result is respectively such as table 2, table 3, table 4
Shown in.
Table 2 is fire resistance and the smoke suppressing data of aluminium hydroxide/zinc microcapsule flame retardant (embodiment 2)
Table 3 is fire resistance and the smoke suppressing data of aluminium hydroxide/zinc microcapsule flame retardant (embodiment 4)
Table 4 is fire resistance and the smoke suppressing data of aluminium hydroxide/zinc microcapsule flame retardant (embodiment 6)
According to table 2, table 3 and table 4 it can be seen that aluminium hydroxide/zinc the microcapsule of the present invention is fire-retardant
Agent has fire resistance and preferably smoke suppressing and the anti-melt-dropping property of excellence to polychloroethylene film material.With
Time, test also finding, this fire retardant is multiple inorganic multiple to polychloroethylene film material mechanical property damage ratio
Join fire retardant little, environment-friendly flame retardant agent can be suitable as.
Claims (10)
1. the preparation method of aluminium hydroxide/zinc microcapsule flame retardant, it is characterised in that include as
Lower step:
1) it is 5～30% aluminum sulfate solution that aluminum sulfate is configured to mass fraction；
2) zinc and dispersant are joined dispersed with stirring in aluminum sulfate solution, obtain mixed liquor；
3) pH value of regulation mixed liquor is 5～9, stirring reaction；Then filter, wash, dried,
Obtain aluminium hydroxide/zinc microcapsule flame retardant.
The preparation method of aluminium hydroxide the most according to claim 1/zinc microcapsule flame retardant, its
Being characterised by, described aluminum sulfate is 2/8～9/1 with the mass ratio of zinc.
The preparation method of aluminium hydroxide the most according to claim 1/zinc microcapsule flame retardant, its
Being characterised by, described dispersant is sodium hexameta phosphate or sodium lauryl sulphate.
The preparation method of aluminium hydroxide the most according to claim 3/zinc microcapsule flame retardant, its
Being characterised by, described dispersant is sodium lauryl sulphate/OP-10.
The preparation method of aluminium hydroxide the most according to claim 4/zinc microcapsule flame retardant, its
Being characterised by, in described dispersant, sodium lauryl sulphate is 2/1～9/1 with the mass ratio of OP-10.
The preparation method of aluminium hydroxide the most according to claim 1/zinc microcapsule flame retardant, its
Being characterised by, the quality of described dispersant is the 0.1～10% of zinc quality.
The preparation method of aluminium hydroxide the most according to claim 1/zinc microcapsule flame retardant, its
Be characterised by, described step 2) in the temperature of dispersed with stirring be 30～70 DEG C.
The preparation method of aluminium hydroxide the most according to claim 1/zinc microcapsule flame retardant, its
Be characterised by, described step 3) in stirring reaction temperature be 40～70 DEG C, the response time is 2～8h.
The preparation method of aluminium hydroxide the most according to claim 1/zinc microcapsule flame retardant, its
Be characterised by, described step 1) in aluminum sulfate is configured to mass fraction is 8～12% aluminum sulfate solution；
Described aluminum sulfate and zinc mass ratio 1～2；Described step 2) in the quality of dispersant be zinc
The 0.4～0.6% of quality；Described step 3) regulation mixed liquor pH value be 6～7, mixing speed
280～320r/min, temperature 50～60 DEG C, the response time 2.8～3.2h.
10. one kind as arbitrary in claim 1～9 as described in the aluminium hydroxide/zinc of preparation method gained micro-
Capsule fire retardant, it is characterised in that the core material of described aluminium hydroxide/zinc microcapsule flame retardant is stannum
Acid zinc, shell material are aluminium hydroxide.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110862574A (en) * | 2019-12-03 | 2020-03-06 | 苏州诺博恩新材料科技有限公司 | Efficient smoke-inhibiting magnesium hydroxide/tin compound microcapsule flame retardant and preparation method thereof |
| CN111205059A (en) * | 2020-03-10 | 2020-05-29 | 河南中柏防火涂料科技有限公司 | Fireproof material with gypsum as base material and construction method thereof |
| CN111233419A (en) * | 2020-03-10 | 2020-06-05 | 河南中柏防火涂料科技有限公司 | Flame-retardant composite material for structure and construction method thereof |
| CN112321890A (en) * | 2020-11-12 | 2021-02-05 | 常州市贝美家居科技有限公司 | Additive for PVC (polyvinyl chloride) plate, PVC plate and preparation method thereof and PVC composite board |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1997000909A1 (en) * | 1995-06-22 | 1997-01-09 | Itri Limited | Fire retardant products |
| CN1948431A (en) * | 2005-10-12 | 2007-04-18 | 中国矿业大学（北京校区） | Preparation method of zinc phosphate cladded aluminium hydroxide composite inorganic fire retardant |
| CN101284993A (en) * | 2008-06-06 | 2008-10-15 | 公安部四川消防研究所 | Nano magnesium hydrate combustion inhibitor using agustite as crystal nucleon component and preparation method |
| CN105060319A (en) * | 2015-07-23 | 2015-11-18 | 韦海棉 | Method for preparing highly-dispersed magnesium hydroxide by magnesium salt |
-
2016
- 2016-04-25 CN CN201610260982.7A patent/CN105860140B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1997000909A1 (en) * | 1995-06-22 | 1997-01-09 | Itri Limited | Fire retardant products |
| CN1948431A (en) * | 2005-10-12 | 2007-04-18 | 中国矿业大学（北京校区） | Preparation method of zinc phosphate cladded aluminium hydroxide composite inorganic fire retardant |
| CN101284993A (en) * | 2008-06-06 | 2008-10-15 | 公安部四川消防研究所 | Nano magnesium hydrate combustion inhibitor using agustite as crystal nucleon component and preparation method |
| CN105060319A (en) * | 2015-07-23 | 2015-11-18 | 韦海棉 | Method for preparing highly-dispersed magnesium hydroxide by magnesium salt |
Non-Patent Citations (1)
| Title |
|---|
| 杨民，等: "羟基锡酸锌包覆氢氧化镁", 《大连交通大学学报》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110862574A (en) * | 2019-12-03 | 2020-03-06 | 苏州诺博恩新材料科技有限公司 | Efficient smoke-inhibiting magnesium hydroxide/tin compound microcapsule flame retardant and preparation method thereof |
| CN111205059A (en) * | 2020-03-10 | 2020-05-29 | 河南中柏防火涂料科技有限公司 | Fireproof material with gypsum as base material and construction method thereof |
| CN111233419A (en) * | 2020-03-10 | 2020-06-05 | 河南中柏防火涂料科技有限公司 | Flame-retardant composite material for structure and construction method thereof |
| CN112321890A (en) * | 2020-11-12 | 2021-02-05 | 常州市贝美家居科技有限公司 | Additive for PVC (polyvinyl chloride) plate, PVC plate and preparation method thereof and PVC composite board |
| CN112321890B (en) * | 2020-11-12 | 2023-06-13 | 常州市贝美家居科技有限公司 | Additive for PVC (polyvinyl chloride) plate, PVC plate, preparation method of PVC plate and PVC composite plate |
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