CN110003529A - The preparation of organically-modified palygorskite and its application in enhancing ethylene-vinyl acetate copolymer anti-flammability - Google Patents

The preparation of organically-modified palygorskite and its application in enhancing ethylene-vinyl acetate copolymer anti-flammability Download PDF

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CN110003529A
CN110003529A CN201910347806.0A CN201910347806A CN110003529A CN 110003529 A CN110003529 A CN 110003529A CN 201910347806 A CN201910347806 A CN 201910347806A CN 110003529 A CN110003529 A CN 110003529A
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acetone
palygorskite
organically
temperature
phthalic anhydride
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杨志旺
花逢林
席辉
李丽
叶娟
魏红
梁习习
张哲�
雷自强
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Northwest Normal University
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/32Phosphorus-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/34Silicon-containing compounds
    • C08K3/346Clay
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/04Oxygen-containing compounds
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    • C08K5/053Polyhydroxylic alcohols
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/04Ingredients treated with organic substances
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/32Phosphorus-containing compounds
    • C08K2003/321Phosphates
    • C08K2003/322Ammonium phosphate
    • C08K2003/323Ammonium polyphosphate
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant

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Abstract

The invention discloses a kind of preparation of organically-modified palygorskite and its applications in enhancing ethylene-vinyl acetate copolymer anti-flammability, preparation: fatty amine is dissolved in acetone, fatty amine acetone soln is obtained, phthalic anhydride is dissolved in acetone, obtains phthalic anhydride acetone soln;Phthalic anhydride acetone soln instills fatty amine acetone soln, circulating condensing mechanic whirl-nett reaction;Palygorskite is added, sufficiently reacts, product is cleaned multiple times in the acetone of product heat, is dried in vacuo, obtains organically-modified palygorskite fire retardant.Preparation method of the present invention utilizes the unique rod-like nano particle structure of palygorskite, it can be improved after organically-modified in the dispersion stabilization of ethylene-vinyl acetate copolymer and the anti-flammability of nanocomposite.

Description

The preparation of organically-modified palygorskite and its enhancing ethylene-vinyl acetate copolymer Application in anti-flammability
Technical field
The invention belongs to fire proofing technical field of surface, it is related to a kind of having using fatty amine and phthalic anhydride The method on machine modified paligorskite surface;The invention further relates to a kind of modified palygorskites in enhancing ethylene-vinyl acetate copolymerization Application in object anti-flammability.
Background technique
Ethylene-vinyl acetate copolymer (EVA) has good elasticity, flexibility, transparency, barrier property, low temperature Toughness, waterproof performance and stable weatherability can also carry out melt-processed, and EVA is compared with rubber, PVC material, almost without gas Taste.In terms of having been applied in many electric materials, especially as electric wire and cable jacket.But EVA material is easily burnt, by A large amount of fire caused by circuit aging shot-firing cable sheath cause researchers to the height weight for preparing EVA fire proofing Depending on.
Palygorskite mineral have unique rod-like nano particle geometry as inorganic fire retardants.With it is other each Anisotropy nano particle is compared, and phyllosilicate pattern is easily controllable, kinetically there is no concern that intercalation or peeling.But it is single Addition palygorskite as fire retardant, flame retardant effect is bad, if palygorskite, which is excessively added, not only will affect fire retardant and polymer Compatibility, and the mechanical property of polymer can be damaged.Recent studies have indicated that organic matter is selected to modify palygorskite, can have The compatibility of the raising palygorskite and basis material of effect, to keep the original mechanical performance of material.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of organically-modified palygorskite, palygorskite and basis material are improved Compatibility, to keep the original mechanical performance of material.
It is a further object to provide a kind of above-mentioned modified paligorskites in enhancing ethylene-vinyl acetate copolymer Application in anti-flammability.
To achieve the above object, the technical scheme adopted by the invention is that: a kind of preparation method of organically-modified palygorskite, Specifically sequentially include the following steps:
1) by 1 ︰ 1~3 of mass ratio, phthalic anhydride and fatty amine are taken respectively;Palygorskite is taken again, and the quality of taken palygorskite is 2~10 times of taken fatty amine quality;
Phthalic anhydride is dissolved completely in acetone, 10~15min is stirred at a temperature of 30~50 DEG C, obtains phthalic acid Acid anhydride acetone soln;
Fatty amine is dissolved completely in acetone, 10~15min is stirred at a temperature of 30~50 DEG C, obtains fatty amine acetone soln;
Fatty amine uses octadecylamine or lauryl amine.
2) phthalic anhydride acetone soln is added dropwise in fatty amine acetone soln, is warming up to 30~70 DEG C, followed Under conditions of ring condensation, the palygorskite that step 1) is taken, 4~10h of mechanical stirring, heat third is added in 2~10h of mechanic whirl-nett reaction Ketone repeatedly washs, and 6~8h is dried in vacuo at a temperature of 20~70 DEG C, obtains organically-modified palygorskite (OPGS).
Another technical solution of the present invention is: the above-mentioned organically-modified palygorskite of one kind is in enhancing ethylene-vinegar Application in vinyl acetate copolymer anti-flammability.Specifically: EVA is added in kneading machine, in 110 DEG C of temperature, the item of revolving speed 60rpm 10min is preheated under part, organically-modified palygorskite is added, is kneaded 15 min, compression template 4min, system are then carried out on vulcanizer Obtain standard batten.(table 1 that the dosage of EVA and organically-modified palygorskite is seen below)
Fire retardant mechanism analysis: in EVA composite material thermal decomposition process, ammonium polyphosphate decomposes the inorganic phosphate compounds generated Catalytic action is played for polymer dehydration carbonization, it is a kind of radical scavenger that inorganic phosphate, which decomposes the PO generated, it can To inhibit polymer to continue to be decomposed into inflammable small-molecule substance in conjunction with the hydrogen atom generated when polymer combustion.Meanwhile it is more Ammonium polyphosphate is thermally decomposed, and nitrogenous inert gas is generated, and the concentration for diluting imflammable gas improves its flame retardant property.EVA base Body material decomposes the layer of charcoal generated and the octadecylamine of modification palygorskite grafting is formed by layer of charcoal, is on the one hand filled out by interface interaction The duct in palygorskite structure is filled, the surface of material is on the other hand coated on by mass action.With increasing for layer of charcoal, protection Layer is thicker, more may advantageously facilitate the extinguishing of flame.
Preparation method of the present invention utilizes the unique rod-like nano particle structure of palygorskite, after organically-modified to palygorskite, Oxygen index (OI) can reach 30.6%, and flame retardant property is relatively preferable.It can be used for industrial production, and lay the foundation for successive modified palygorskite.
Detailed description of the invention
Fig. 1 is the infrared comparison diagram of the present invention organically-modified palygorskite and palygorskite original soil.
Fig. 2 is the comparison diagram on the surface that the basis material EVA palygorskite modified with the present invention compounds.
Specific embodiment
To carry out the processing technique of palygorskite surface organic modification of the present invention below by specific example more detailed Step explanation.
Embodiment 1
5g phthalic anhydride is dissolved completely in acetone, stirs 10min at a temperature of 30 DEG C, and it is molten to obtain phthalic anhydride acetone Liquid;6g octadecylamine is dissolved completely in acetone, stirs 10min at a temperature of 50 DEG C, obtains octadecylamine acetone soln;By phthalic acid Acid anhydride acetone soln is added dropwise in octadecylamine acetone soln, under conditions of circulating condensing, after mechanic whirl-nett reaction 4h;It is added 20g palygorskite, mechanical stirring 6h;It is cleaned multiple times with the acetone of heat, dry 6h at a temperature of 50 DEG C, obtains organic change in vacuum drying oven The palygorskite of property.
The infrared spectroscopy of organically-modified palygorskite (OPGS) and unmodified palygorskite (PGS) obtained in embodiment 1 Figure, is shown in Fig. 1.In the infrared spectrogram of palygorskite (PGS), 3610cm-1With 1636 cm-1Place occur palygorskite (Al, Mg) the hydroxyl stretching vibration absworption peak of-OH.In the infrared spectrogram of organically-modified palygorskite, OPGS is in 1030 cm-1Locate peak Intensity obviously weakens, and can illustrate that Si-O-Si and Al-O-Si structure has been destroyed accordingly, indirect proof phthalic anhydride and ten Eight amine, which have occurred, occurs acylation reaction with palygorskite surface.In addition, the infrared light spectral peak of OPGS is in 2983 cm-1、2889 cm-1 There are two peaks newly increased in place, be methylene symmetrically and asymmetric stretching vibration absworption peak.Prove phthalic anhydride and Octadecylamine and the carboxyl on palygorskite surface react, and have successfully been grafted to palygorskite surface.
Pure palygorskite and embodiment 1 obtain it is organically-modified after palygorskite surface topography map, as shown in Figure 2.From Fig. 2 In as can be seen that pure palygorskite surface smoother (Fig. 2 a), repaired with phthalic anhydride and octadecylamine acylation reaction product Palygorskite after decorations, surface are uniformly covered with one layer of white organic matter (Fig. 2 b).This illustrates phthalic anhydride and 18 Amine acylate is grafted to palygorskite surface.Phthalic anhydride and the organically-modified palygorskite of octadecylamine acyl are embodied in matrix There is good compatibility in material.
Embodiment 2
5g phthalic anhydride is dissolved completely in acetone, 30 DEG C at a temperature of stir 12min, obtain phthalic anhydride acetone Solution;6g octadecylamine is dissolved completely in acetone, 45 DEG C at a temperature of stir 12min, obtain octadecylamine acetone soln;By adjacent benzene Dicarboxylic acid anhydride acetone soln is added dropwise in octadecylamine acetone soln, under conditions of circulating condensing, after mechanic whirl-nett reaction 4h; 20g palygorskite, mechanical stirring 6h is added, hot acetone is cleaned multiple times product, in 50 DEG C of at a temperature of dry 6h in vacuum drying oven, Obtain organically-modified palygorskite.
Embodiment 3
7g phthalic anhydride is dissolved completely in acetone, stirs 15min at a temperature of 30 DEG C, and it is molten to obtain phthalic anhydride acetone Liquid;12g octadecylamine is dissolved completely in acetone, stirs 15min at a temperature of 40 DEG C, obtains octadecylamine acetone soln;By adjacent benzene two Formic anhydride acetone soln is added dropwise in octadecylamine acetone soln, under conditions of circulating condensing, after mechanic whirl-nett reaction 3h;Add Enter 24g palygorskite, mechanical stirring 6h, hot acetone is cleaned multiple times product, and dry 8h at a temperature of 20 DEG C, must have in vacuum drying oven Machine modified paligorskite.
Embodiment 4
7g phthalic anhydride is dissolved completely in acetone, 30 DEG C at a temperature of stir 12min, obtain phthalic anhydride acetone Solution;12g octadecylamine is dissolved completely in acetone, 35 DEG C at a temperature of stir 15min, obtain octadecylamine acetone soln;It will be adjacent Phthalate anhydride acetone soln is added dropwise in octadecylamine acetone soln, under conditions of circulating condensing, mechanic whirl-nett reaction 3h Afterwards;120g palygorskite, mechanical stirring 4h is added, hot acetone is cleaned multiple times product, dry 6h at a temperature of 70 DEG C in vacuum drying oven, Obtain organically-modified palygorskite.
Embodiment 5
7g phthalic anhydride is dissolved completely in acetone, stirs 10min at a temperature of 30 DEG C, and it is molten to obtain phthalic anhydride acetone Liquid;18.2g octadecylamine is dissolved completely in acetone, stirs 12min at a temperature of 30 DEG C, obtains octadecylamine acetone soln;By adjacent benzene two Formic anhydride acetone soln is added dropwise in octadecylamine acetone soln, under conditions of circulating condensing, mechanic whirl-nett reaction 10h;Add Enter 36.4g palygorskite, mechanical stirring 7h, hot acetone is cleaned multiple times, and dry 6.5h at a temperature of 60 DEG C, must have in vacuum drying oven Machine modified paligorskite.
Embodiment 6
7g phthalic anhydride is dissolved completely in acetone, stirs 12min at a temperature of 35 DEG C, and it is molten to obtain phthalic anhydride acetone Liquid;18g octadecylamine is dissolved completely in acetone, stirs 10min at a temperature of 50 DEG C, obtains octadecylamine acetone soln;By adjacent benzene two Formic anhydride acetone soln is added dropwise in octadecylamine acetone soln, under conditions of circulating condensing, mechanic whirl-nett reaction 2h;It is added 54g palygorskite, mechanical stirring 8h, hot acetone are cleaned multiple times product, and dry 6h at a temperature of 30 DEG C, obtains organic in vacuum drying oven Modified paligorskite.
Embodiment 7
9g phthalic anhydride is dissolved completely in acetone, stirs 15min at a temperature of 35 DEG C, and it is molten to obtain phthalic anhydride acetone Liquid;18g octadecylamine is dissolved completely in acetone, stirs 12min at a temperature of 45 DEG C, obtains octadecylamine acetone soln;By adjacent benzene two Formic anhydride acetone soln is added dropwise in octadecylamine acetone soln, under conditions of circulating condensing, after mechanic whirl-nett reaction 9h;Add Enter 54g palygorskite, mechanical stirring 6h, product is cleaned multiple times in hot acetone, and 40 DEG C of drying 6h in vacuum drying oven obtain organically-modified slope Thread stone.
Embodiment 8
9g phthalic anhydride is dissolved completely in acetone, stirs 12min at a temperature of 35 DEG C, and it is molten to obtain phthalic anhydride acetone Liquid;18g octadecylamine is dissolved completely in acetone, stirs 10min at a temperature of 40 DEG C, obtains octadecylamine acetone soln;By adjacent benzene two Formic anhydride acetone soln is added dropwise in octadecylamine acetone soln, under conditions of circulating condensing, mechanic whirl-nett reaction 8h;It is added 90g palygorskite, mechanical stirring 8h, hot acetone are cleaned multiple times product, and dry 7h at a temperature of 60 DEG C, obtains organic in vacuum drying oven Modified paligorskite.
Embodiment 9
9g phthalic anhydride is dissolved completely in acetone, stirs 12min at a temperature of 35 DEG C, and it is molten to obtain phthalic anhydride acetone Liquid;21g octadecylamine is dissolved completely in acetone, stirs 15min at a temperature of 35 DEG C, obtains octadecylamine acetone soln;By adjacent benzene two Formic anhydride acetone soln is added dropwise in octadecylamine acetone soln, under conditions of circulating condensing, after mechanic whirl-nett reaction 2h;Add Entering 42g palygorskite, mechanical stirring 10h, hot acetone is cleaned multiple times product, dry 7.5h at a temperature of 30 DEG C in vacuum drying oven, Obtain organically-modified palygorskite.
Embodiment 10
9g phthalic anhydride is dissolved completely in acetone, stirs 12min at a temperature of 40 DEG C, and it is molten to obtain phthalic anhydride acetone Liquid;21g octadecylamine is dissolved completely in acetone, stirs 10min at a temperature of 50 DEG C, obtains octadecylamine acetone soln;By adjacent benzene two Formic anhydride acetone soln is added dropwise in octadecylamine acetone soln, under conditions of circulating condensing, after mechanic whirl-nett reaction 5h;Add Enter 126g palygorskite, mechanical stirring 6h, hot acetone is cleaned multiple times product, and dry 8h at a temperature of 60 DEG C, obtains in vacuum drying oven Organically-modified palygorskite.
Embodiment 11
11g phthalic anhydride is dissolved completely in acetone, stirs 12min at a temperature of 40 DEG C, obtains phthalic anhydride acetone Solution;21g octadecylamine is dissolved completely in acetone, stirs 15min at a temperature of 45 DEG C, obtains octadecylamine acetone soln;By adjacent benzene Dicarboxylic acid anhydride acetone soln is added dropwise in octadecylamine acetone soln, under conditions of circulating condensing, after mechanic whirl-nett reaction 9h; 147g palygorskite, mechanical stirring 8h is added, hot acetone is cleaned multiple times product, dry 6h at a temperature of 70 DEG C in vacuum drying oven, Obtain organically-modified palygorskite.
Embodiment 12
11g phthalic anhydride is dissolved completely in acetone, stirs 10min at a temperature of 40 DEG C, obtains phthalic anhydride acetone Solution;21g octadecylamine is dissolved completely in acetone, stirs 15min at a temperature of 40 DEG C, obtains octadecylamine acetone soln;By adjacent benzene Dicarboxylic acid anhydride acetone soln is added dropwise in octadecylamine acetone soln, under conditions of circulating condensing, after mechanic whirl-nett reaction 8h; 168g palygorskite is added, product is cleaned multiple times with the acetone of heat in mechanical stirring 10h, dry at a temperature of 40 DEG C in vacuum drying oven 6h obtains organically-modified palygorskite.
Embodiment 13
11g phthalic anhydride is dissolved completely in acetone, stirs 10min at a temperature of 40 DEG C, obtains phthalic anhydride acetone Solution;21g octadecylamine is dissolved completely in acetone, stirs 12min at a temperature of 35 DEG C, obtains octadecylamine acetone soln;By adjacent benzene Dicarboxylic acid anhydride acetone soln is added dropwise in octadecylamine acetone soln, under conditions of circulating condensing, after mechanic whirl-nett reaction 7h; 189g palygorskite, mechanical stirring 8h is added, hot acetone is cleaned multiple times product, dry 7h at a temperature of 70 DEG C in vacuum drying oven, Obtain organically-modified palygorskite.
Embodiment 14
13g phthalic anhydride is dissolved completely in acetone, stirs 10min at a temperature of 40 DEG C, obtains phthalic anhydride acetone Solution;21g octadecylamine is dissolved completely in acetone, stirs 10min at a temperature of 30 DEG C, obtains octadecylamine acetone soln;By adjacent benzene Dicarboxylic acid anhydride acetone soln is added dropwise in octadecylamine acetone soln, under conditions of circulating condensing, mechanic whirl-nett reaction 6h;Add Enter 210g palygorskite, mechanical stirring 7h, hot acetone is cleaned multiple times product, and dry 6h at a temperature of 50 DEG C, obtains in vacuum drying oven Organically-modified palygorskite.
Embodiment 15
13g phthalic anhydride is dissolved completely in acetone, stirs 12min at a temperature of 45 DEG C, obtains phthalic anhydride acetone Solution;21g octadecylamine is dissolved completely in acetone, stirs 10min at a temperature of 50 DEG C, obtains octadecylamine acetone soln;By adjacent benzene Dicarboxylic acid anhydride acetone soln is added dropwise in octadecylamine acetone soln, under conditions of circulating condensing, mechanic whirl-nett reaction 4h;Add Enter 42g palygorskite, mechanical stirring 6h, hot acetone is cleaned multiple times product, and dry 7h at a temperature of 70 DEG C, must have in vacuum drying oven Machine modified paligorskite.
Embodiment 16
13g phthalic anhydride is dissolved completely in acetone, stirs 12min at a temperature of 45 DEG C, obtains phthalic anhydride acetone Solution;26g octadecylamine is dissolved completely in acetone, stirs 10min at a temperature of 45 DEG C, obtains octadecylamine acetone soln;By adjacent benzene Dicarboxylic acid anhydride acetone soln is added dropwise in octadecylamine acetone soln, under conditions of circulating condensing, mechanic whirl-nett reaction 2h;Add Enter 69g palygorskite, mechanical stirring 6h, hot acetone is cleaned multiple times product, and dry 8h at a temperature of 45 DEG C, must have in vacuum drying oven Machine modified paligorskite.
Embodiment 17
13g phthalic anhydride is dissolved completely in acetone, stirs 15min at a temperature of 45 DEG C, obtains phthalic anhydride acetone Solution;39g octadecylamine is dissolved completely in acetone, stirs 12min at a temperature of 40 DEG C, obtains octadecylamine acetone soln;By adjacent benzene Dicarboxylic acid anhydride acetone soln is added dropwise in octadecylamine acetone soln, under conditions of circulating condensing, mechanic whirl-nett reaction 10h Afterwards;156g palygorskite, mechanical stirring 8h is added, hot acetone is cleaned multiple times product, dry at a temperature of 60 DEG C in vacuum drying oven 6h obtains organically-modified palygorskite.
Embodiment 18
15g phthalic anhydride is dissolved completely in acetone, stirs 10min at a temperature of 45 DEG C, obtains phthalic anhydride acetone Solution;23g octadecylamine is dissolved completely in acetone, stirs 10min at a temperature of 35 DEG C, obtains octadecylamine acetone soln;By adjacent benzene Dicarboxylic acid anhydride acetone soln is added dropwise in octadecylamine acetone soln, under conditions of circulating condensing, mechanic whirl-nett reaction 6h;Add Enter 115g palygorskite, mechanical stirring 6h, hot acetone is cleaned multiple times product, and dry 6h at a temperature of 50 DEG C, obtains in vacuum drying oven Organically-modified palygorskite.
Embodiment 19
15g phthalic anhydride is dissolved completely in acetone, stirs 12min at a temperature of 45 DEG C, obtains phthalic anhydride acetone Solution;23g lauryl amine is dissolved completely in acetone, stirs 10min at a temperature of 30 DEG C, obtains lauryl amine acetone soln;By adjacent benzene Dicarboxylic acid anhydride acetone soln is added dropwise in lauryl amine acetone soln, under conditions of circulating condensing, after mechanic whirl-nett reaction 7h; 230g palygorskite, mechanical stirring 6h is added, hot acetone is cleaned multiple times product, dry 6h at a temperature of 70 DEG C in vacuum drying oven, Obtain organically-modified palygorskite.
Embodiment 20
17g phthalic anhydride is dissolved completely in acetone, stirs 10min at a temperature of 50 DEG C, obtains phthalic anhydride acetone Solution;23g lauryl amine is dissolved completely in acetone, stirs 12min at a temperature of 50 DEG C, obtains lauryl amine acetone soln;By adjacent benzene Dicarboxylic acid anhydride acetone soln is added dropwise in lauryl amine acetone soln, under conditions of circulating condensing, mechanic whirl-nett reaction 8h;Add Enter 46g palygorskite, mechanical stirring 6h, hot acetone is cleaned multiple times product, and dry 6h at a temperature of 50 DEG C, must have in vacuum drying oven Machine modified paligorskite.
Embodiment 21
17g phthalic anhydride is dissolved completely in acetone, stirs 12min at a temperature of 50 DEG C, obtains phthalic anhydride acetone Solution;23g lauryl amine is dissolved completely in acetone, stirs 15min at a temperature of 45 DEG C, obtains lauryl amine acetone soln;By adjacent benzene Dicarboxylic acid anhydride acetone soln is added dropwise in lauryl amine acetone soln, under conditions of circulating condensing, mechanic whirl-nett reaction 4h;Add Enter 69g palygorskite, mechanical stirring 6h, hot acetone is cleaned multiple times product, and dry 6h at a temperature of 20 DEG C, must have in vacuum drying oven Machine modified paligorskite.
Organically-modified palygorskite (OPGS) made from the various embodiments described above is made after compounding with ammonium polyphosphate and pentaerythrite For fire retardant be applied to ethylene-vinyl acetate copolymer (EVA) basis material in, the LOI value of obtained composite material with UL-94 value, as shown in table 1.
LOI and the UL-94 data of table 1EVA and EVA composite material
As can be seen from Table 1: in the EVA basis material that 3wt% OPGS and 30wt%APP/PER are added to 70 wt%, obtaining The oxygen index (OI) of composite material reaches peak 30.6%, and oxygen index (OI) is higher, illustrates the fire-retardant of organically-modified Palygorskite Composite Materials Property is relatively preferable.
EVA and fire-retardant EVA composite material are in the APP/PER/OPGS (3%) and APP/PER/PGS for adding 30wt% specific gravity (3%) mechanical performance data.As shown in table 2.
Table 2EVA composite materials property data
Table 2 shows that the tensile strength of EVA/APP/PER/OPGS (3%), elongation at break ratio EVA/APP/PER/PGS (3%) are equal It increases.Its mechanical property is better than unmodified Palygorskite Composite Materials.

Claims (3)

1. a kind of preparation method of organically-modified palygorskite, specifically sequentially includes the following steps:
1) by 1 ︰ 1~3 of mass ratio, phthalic anhydride and fatty amine are taken respectively;Palygorskite is taken again, and the quality of taken palygorskite is 2~10 times of taken fatty amine quality;
Phthalic anhydride is dissolved completely in acetone, 10~15min is stirred at a temperature of 30~50 DEG C, obtains phthalic acid Acid anhydride acetone soln;
Fatty amine is dissolved completely in acetone, 10~15min is stirred at a temperature of 30~50 DEG C, obtains fatty amine acetone soln;
2) phthalic anhydride acetone soln is added dropwise in fatty amine acetone soln, is warming up to 30~70 DEG C, it is cold recycling Under conditions of solidifying, 2~10h of mechanic whirl-nett reaction is added the palygorskite that step 1) is taken, 4~10h of mechanical stirring, and hot acetone is more Secondary washing is dried in vacuo 6~8h at a temperature of 20~70 DEG C, obtains organically-modified palygorskite (OPGS).
2. the preparation method of organically-modified palygorskite as described in claim 1, which is characterized in that the fatty amine uses 12 Amine or octadecylamine.
3. organically-modified palygorskite made from a kind of preparation method described in claim 1 enhancing ethylene-vinyl acetate Application in copolymer anti-flammability.
CN201910347806.0A 2019-04-28 2019-04-28 The preparation of organically-modified palygorskite and its application in enhancing ethylene-vinyl acetate copolymer anti-flammability Pending CN110003529A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105330561A (en) * 2014-08-12 2016-02-17 上海华明高技术(集团)有限公司 Calcium carbonate surface modifier as well as composition of calcium carbonate and modifier and preparation method thereof
CN107868281A (en) * 2017-11-28 2018-04-03 西北师范大学 A kind of preparation of hypo-aluminum orthophosphate doping vario-property palygorskite and the application as fire retardant

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105330561A (en) * 2014-08-12 2016-02-17 上海华明高技术(集团)有限公司 Calcium carbonate surface modifier as well as composition of calcium carbonate and modifier and preparation method thereof
CN107868281A (en) * 2017-11-28 2018-04-03 西北师范大学 A kind of preparation of hypo-aluminum orthophosphate doping vario-property palygorskite and the application as fire retardant

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