CN108102145A - Preparation method of load type hydrotalcite-based flame retardant and heat stabilizer and PVC product - Google Patents
Preparation method of load type hydrotalcite-based flame retardant and heat stabilizer and PVC product Download PDFInfo
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- CN108102145A CN108102145A CN201711345275.9A CN201711345275A CN108102145A CN 108102145 A CN108102145 A CN 108102145A CN 201711345275 A CN201711345275 A CN 201711345275A CN 108102145 A CN108102145 A CN 108102145A
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- heat stabilizer
- retardant
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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
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
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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
- C08K3/26—Carbonates; Bicarbonates
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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
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
the invention provides a preparation method of a load type hydrotalcite-based flame retardant and heat stabilizer and a PVC product, wherein the preparation method comprises the following steps of dissolving 4.5-7.5 parts of a surface modifier in absolute ethyl alcohol, then putting 100-120 parts of magnesium-aluminum hydrotalcite and 30-50 parts of brucite into a ball milling tank, grinding for 0.5-3 h at a ball milling rotating speed of 200-500r/min, and drying in a drying box to obtain the load type hydrotalcite-based flame retardant and heat stabilizer.
Description
Technical field
The present invention relates to the technical field for improving PVC anti-flammabilitys and thermal stability, more particularly to a kind of carried hydrotalcites
Base is fire-retardant and heat stabilizer and preparation method thereof.
Background technology
Polyvinyl chloride（PVC）It is one of plastics variety for realizing industrialized production earliest in the world, is occupied in global demand amount
The 3rd is occupied after polyethylene, polypropylene.PVC product has hardness easy-regulating, high mechanical properties, corrosion-resistant, electrical insulating property
Good, transparent high, wear-resisting, fire retardant, self-extinguishment and it is inexpensive the advantages that, in building, light industry, chemical industry, electronics, space flight, automobile, agricultural
Have been widely used etc. having in many fields.But due to the fault of construction of PVC, it is being heated, shearing or is being subject to high-energy rays
Degradation and cross-linking reaction easily occur under the influence of (such as ultraviolet light), causes to process and using difficulty, the color burn of product, mechanics
Hydraulic performance decline；The corrosive gas such as substantial amounts of black smoke and HCl, CO can be generated in fire burning.According to statistics, in fire incident
Personnel's cause of death more than 80% is related with dense smoke and toxic gas that material generates, drastically influences the life and property of people
Safety.Therefore, in PVC process, the method for the generally use addition auxiliary agents such as fire retardant and heat stabilizer, to improve PVC
The melt strength of resin reduces processing temperature, improves the presentation quality of product, while improves the flame retardant property of PVC, reduces burning
Smoke amount in the process, application and raising Product Safety to PVC are of great significance.
The fire retardant of PVC mainly includes machine fire retardant and inorganic combustion inhibitor, organic fire-retardant in PVC using less,
What general PVC matrix was selected is all inorganic combustion inhibitor.Inorganic combustion inhibitor can be divided into metal hydroxides, antimony system, tin system, boron system
Deng.Metal hydroxide combustion inhibitor derives from a wealth of sources, is cheap, mainly includes aluminium hydroxide and magnesium hydroxide.When being heated to heat
It is decomposed when solving temperature, releases the crystallization water, absorb substantial amounts of heat, so as to reduce the temperature of polymer surfaces, delay high polymer
Thermal degradation speed, slow down or inhibit the burning of high polymer, and promote to carbonize, it is dense that the vapor released can dilute combustible
Degree reduces contribution of the combustible to burning, and system thermal discharge and smoke amount is caused to reduce, makes flameout.
There are many PVC heat stabilizer species, can be divided into lead salts, metal soap, organic tin, antimony organic according to chemical composition
Class, terres rares, organic auxiliary heat stabilizer, composite thermal stabilizer and hydrotalcite heat stabilizer.Wherein it is most of be it is toxic,
This not only limits the application range of PVC product, and can damage in use to environment and work health.In recent years
Come the European, U.S., Japan and China successively to formulate and implement policy and regulation of the limitation using poisonous and harmful chemicals,
Therefore the inorganic heat stabilizer of environmental type becomes the emphasis of research.
The content of the invention
The present invention in view of the above shortcomings of the prior art, propose that a kind of carried hydrotalcite base is fire-retardant and heat stabilizer and
The preparation method of PVC product.
The technical scheme is that realize in the following manner：A kind of carried hydrotalcite base is fire-retardant and heat stabilizer
Preparation method carries out in the following manner：4.5 ~ 7.5 parts of surface modifiers are dissolved in absolute ethyl alcohol, afterwards with 100 ~
120 parts of magnalium hydrotalcites, 30 ~ 50 parts of shepardites are put into ball grinder, and 0.5h-3h is ground with 200-500r/min rotational speed of ball-mill；
It is dried afterwards in drying box, obtains that carried hydrotalcite base is fire-retardant and heat stabilizer.
The surface modifier is aluminum stearate either odium stearate or lauric acid.
The surface modifier is with absolute ethyl alcohol according to 1g:The ratio of 10-15mL is dissolved.
Ratio of grinding media to material in the ball grinder is 30 ~ 60:1.
Drying is to dry 2h in 80 DEG C of electric drying oven with forced convection in the drying box.
The method that carried hydrotalcite base is fire-retardant and heat stabilizer prepares PVC product, carries out in the following manner：It will
Above-mentioned carried hydrotalcite base is fire-retardant and heat stabilizer with PVC according to 10-30：100 mass ratio after mixing, adds matter
The o-2-octyl that amount fraction is 10% is uniformly mixed, and mixed material is put into 100 DEG C of baking oven and dries 2h, through injection molding machine
Or double screw extruder is pressed into product.
The carried hydrotalcite base of the present invention is fire-retardant and heat stabilizer has the following advantages：
1st, PVC thermal stability is significantly improved, including static heat stability energy, dynamic thermal stability energy and remaining thermal stability.
2nd, the flame-proof smoke-suppressing of PVC, oxygen index (OI) are significantly improved（LOI）It significantly improves.
3rd, it is green safe, it is nontoxic, it is good with PVC matrix compatibility.
4th, at low cost, raw material sources are extensive, and preparation process is simple.
Description of the drawings
Fig. 1 is congo red method experimental rig figure.
Specific embodiment
Below in conjunction with the attached drawing in the embodiment of the present invention, the technical solution in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other under the premise of not making the creative labor
Embodiment belongs to the scope of protection of the invention.
Carried hydrotalcite base is fire-retardant and the preparation method of heat stabilizer, carries out in the following manner：By 4.5 ~ 7.5
Part surface modifier is dissolved in absolute ethyl alcohol, is put into ball grinder with 100 ~ 120 parts of magnalium hydrotalcites, 30 ~ 50 parts of shepardites afterwards
In, in planetary ball mill, 0.5h-3h is ground with 200-500r/min rotational speed of ball-mill.
The surface modifier is with absolute ethyl alcohol according to 1g:The ratio of 10-15mL is dissolved.
The surface modifier is aluminum stearate either odium stearate or lauric acid.
Ratio of grinding media to material in the ball grinder is 30 ~ 60:1.
The method that the carried hydrotalcite base is fire-retardant and heat stabilizer prepares PVC product is to hinder the PVC of above-mentioned preparation
Combustion and heat stabilizer and PVC are according to 10-30：100 mass ratio obtains mixture after mixing, and it is upper to add mass fraction
The o-2-octyl for stating mixture 10% is uniformly mixed, and mixed material is put into 100 DEG C of baking oven and dries 2h, through injection molding machine
Or double screw extruder is pressed into product.
Embodiment 1：
It weighs 6g aluminum stearates to be dissolved in 75mL absolute ethyl alcohols, 100g magnalium hydrotalcites and 50g shepardites is put into 250mL together
In ball grinder, ratio of grinding media to material 50:1, mechano-chemical reation is carried out, the ball milling 1h under the rotating speed of 300r/min takes out product,
2h is dried in 80 DEG C of electric drying oven with forced convection, obtains that carried hydrotalcite base is fire-retardant and heat stabilizer, the fire-retardant and thermostabilization help
Agent is added to the dosage of 30wt.% in PVC, can the heat-stable time of PVC be increased to 82min by 12min, oxygen index (OI) by
25.5% is increased to 35.8%.
Embodiment 2：
It weighs 7.5g odium stearate to be dissolved in 90mL absolute ethyl alcohols, 120g magnalium hydrotalcites and 30 shepardites is put into together
In 250mL ball grinders, ratio of grinding media to material 40:1, mechano-chemical reation is carried out, the ball milling 2h under the rotating speed of 200r/min takes out production
Product dry 2h in 80 DEG C of electric drying oven with forced convection, obtain that carried hydrotalcite base is fire-retardant and heat stabilizer, this is fire-retardant and hot steady
Determine auxiliary agent with the dosage of 20wt.% to be added in PVC, the heat-stable time of PVC can be increased to 80min, oxygen index (OI) by 12min
35% is increased to by 25.5%.
Embodiment 3：
It weighs 5g lauric acid to be dissolved in 60mL absolute ethyl alcohols, 100g magnalium hydrotalcites and 50g shepardites is put into 250mL balls together
In grinding jar, ratio of grinding media to material 30:1, mechano-chemical reation is carried out, the ball milling 0.5h under the rotating speed of 500r/min takes out product,
2h is dried in 80 DEG C of electric drying oven with forced convection, obtains that carried hydrotalcite base is fire-retardant and heat stabilizer, the fire-retardant and thermostabilization help
Agent is added to the dosage of 15wt.% in PVC, can the heat-stable time of PVC be increased to 78min by 12min, oxygen index (OI) by
25.5% is increased to 34.7%.
Embodiment 4：
It weighs 7g aluminum stearates to be dissolved in 80mL absolute ethyl alcohols, 110g magnalium hydrotalcites and 40g shepardites is put into 250mL together
In ball grinder, ratio of grinding media to material 50:1, mechano-chemical reation is carried out, the ball milling 1h under the rotating speed of 300r/min takes out product,
2h is dried in 80 DEG C of electric drying oven with forced convection, obtains that carried hydrotalcite base is fire-retardant and heat stabilizer, the fire-retardant and thermostabilization help
Agent is added to the dosage of 25wt.% in PVC, can the heat-stable time of PVC be increased to 85min by 12min, oxygen index (OI) by
25.5% is increased to 36%.
Embodiment 5
It weighs 6.5g odium stearate to be dissolved in 65mL absolute ethyl alcohols, 105g magnalium hydrotalcites and 45g shepardites is put into together
In 250mL ball grinders, ratio of grinding media to material 40:1, mechano-chemical reation is carried out, 1 ~ 3h of ball milling under the rotating speed of 300r/min takes out
Product dries 2h in 80 DEG C of electric drying oven with forced convection, obtains that carried hydrotalcite base is fire-retardant and heat stabilizer, this is fire-retardant and hot
Stabilization aid is added to the dosage of 30wt.% in PVC, can the heat-stable time of PVC be increased to 75min by 12min, oxygen refers to
Number is increased to 32.7% by 25.5%.
Embodiment 6
It weighs 4.5g lauric acid to be dissolved in 60mL absolute ethyl alcohols, 100g magnalium hydrotalcites and 40g shepardites is put into 250mL together
In ball grinder, ratio of grinding media to material 30:1, mechano-chemical reation is carried out, the ball milling 1h under the rotating speed of 500r/min takes out product,
2h is dried in 80 DEG C of electric drying oven with forced convection, obtains that carried hydrotalcite base is fire-retardant and heat stabilizer, the fire-retardant and thermostabilization help
Agent is added to the dosage of 15wt.% in PVC, can the heat-stable time of PVC be increased to 76min by 12min, oxygen index (OI) by
25.5% is increased to 35.2%.
In the application, the measuring method of PVC heat-stable times：
Congo red method：According to GB/T 2917.1-2002《Blend and product based on ryuron and copolymer exist
Hydrogen chloride and measure-congo red method of any other acid product are released during high temperature》It performs.Concrete operations are as follows：By PVC product
Cutting makes more than 80% material sieve (GB/T 6003) by 2.0 mm and is stayed in and most of material on 1.4 mm sieves, with 1.4
Mm residue on sieves prepare sample.The sample 6 of preparation is put into test tube 1, about 50 mm of height, slight vibration should not fill sample
It crosses reality or is sticked on test tube wall.2 one end of Congored test paper is rolled or is folded for insertion into thin glass tube 3, thin glass tube is inserted into
In plug 4, test tube is clogged with plug, and adjusts position of the glass tube in plug so that the bottom of test paper is away from sample surface 25
mm.The immersion of ready test tube has been reached to the oil bath 5 of test temperature (180 DEG C)（Place heat insulation layer 7 in the top of oil bath 5）In to try
Sample surface sustained height starts timing.When significantly from red to blue indicating occurs in the Congored test paper 2 in test tube, stop meter
When.Using the arithmetic mean of instantaneous value of result of the parallel determination based on dividing as stabilization time.When the relative deviation of single value and average value is big
When 10%, result should be abandoned and redeterminated.Its experimental rig figure is as shown in Figure 1.
PVC limiting oxygen index determinations in the application：
Specimen size used in limiting oxygen index determination is 100mm × 6.5mm × 3mm, by GB2406-80 standards, utilizes the types of XZT -100
Oxygen index instrument detects the combustibility of sample.
Rule of thumb or sample situation about lighting in air, estimation start oxygen concentration during experiment.Specimen holder is being pressed from both sides
On tool, the center of combustion barrel is vertically installed at, ensures sample top less than combustion barrel top at least 100mm, exposure
Part lowest part should be higher than that combustion barrel bottom air distributing device top at least 100mm.Adjusting gas flow control device, make oxygen and
The oxygen concentration that oxygen concentration in the mixed gas of nitrogen measures when being and starting, and combustion barrel is flowed through with the speed of 40 ± 10mm/s,
Wash combustion barrel at least 30s.Fully reduction and mobile igniter, makes flame visible part be applied to sample top surface, simultaneously
It is applied to perpendicular lateral wall profile about 6mm long.When lighting sample, flame interaction time up to 30s.Igniting is slightly removed every 5s or so
Device observes sample, until perpendicular lateral wall profile stablizes burning or the forward of visible combustion part is reached at upper graticule, removes immediately a little
Firearm starts timing or observation sample burning length.If sample cannot be lighted in 30s, increase oxygen concentration, light again, directly
Until being lighted in 30s.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modifications, equivalent replacements and improvements are made should all be included in the protection scope of the present invention god.
Claims (6)
1. carried hydrotalcite base is fire-retardant and the preparation method of heat stabilizer, it is characterised in that carries out in the following manner：
4.5 ~ 7.5 parts of surface modifiers are dissolved in absolute ethyl alcohol, are put afterwards with 100 ~ 120 parts of magnalium hydrotalcites, 30 ~ 50 parts of shepardites
Enter in ball grinder, 0.5h-3h is ground with 200-500r/min rotational speed of ball-mill；It is dried afterwards in drying box, obtains support type water
Talcum base is fire-retardant and heat stabilizer.
2. carried hydrotalcite base according to claim 1 is fire-retardant and the preparation method of heat stabilizer, it is characterised in that：Institute
It is aluminum stearate either odium stearate or lauric acid to state surface modifier.
3. carried hydrotalcite base according to claim 1 or 2 is fire-retardant and the preparation method of heat stabilizer, feature exist
In：The surface modifier is with absolute ethyl alcohol according to 1g:The ratio of 10-15mL is dissolved.
4. carried hydrotalcite base according to claim 1 or 2 is fire-retardant and the preparation method of heat stabilizer, feature exist
In：Ratio of grinding media to material in the ball grinder is 30 ~ 60:1.
5. carried hydrotalcite base according to claim 1 or 2 is fire-retardant and the preparation method of heat stabilizer, feature exist
In：Drying is to dry 2h in 80 DEG C of electric drying oven with forced convection in the drying box.
The method that 6. carried hydrotalcite base is fire-retardant and heat stabilizer prepares PVC product, it is characterised in that be in the following manner
It carries out：By the carried hydrotalcite base obtained by claim 1 ~ 4 is fire-retardant and heat stabilizer with PVC according to 10-30：100 matter
It measures ratio after mixing, adds the o-2-octyl that mass fraction is 10% and be uniformly mixed, mixed material is put into 100
DEG C baking oven in dry 2h, be pressed into product through injection molding machine or double screw extruder.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108690257A (en) * | 2018-06-05 | 2018-10-23 | 海南鸿昌兴科技股份有限公司 | The non-crosslinked polyolefin composition of heat-resistant halogen-free low-smoke and flame retardant for cable |
| CN113831590A (en) * | 2021-10-20 | 2021-12-24 | 江西广源化工有限责任公司 | Flame-retardant smoke-suppressing mineral complex and preparation method and application thereof |
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| CN113831590A (en) * | 2021-10-20 | 2021-12-24 | 江西广源化工有限责任公司 | Flame-retardant smoke-suppressing mineral complex and preparation method and application thereof |
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