CN108841048A - A kind of dedicated low smell in floor is without phenol calcium zinc stabilizer and preparation method thereof - Google Patents

A kind of dedicated low smell in floor is without phenol calcium zinc stabilizer and preparation method thereof Download PDF

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Publication number
CN108841048A
CN108841048A CN201810585755.0A CN201810585755A CN108841048A CN 108841048 A CN108841048 A CN 108841048A CN 201810585755 A CN201810585755 A CN 201810585755A CN 108841048 A CN108841048 A CN 108841048A
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stabilizer
low smell
calcium zinc
floor
antioxidant
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沈卫锋
徐良坤
杨振华
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Jiangsu Carinver Technology Co Ltd
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Jiangsu Carinver Technology Co Ltd
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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
    • C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/04—Ingredients characterised by their shape and organic or inorganic ingredients
    • 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
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C08K3/042—Graphene or derivatives, e.g. graphene oxides
    • 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
    • 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
    • C08K3/32—Phosphorus-containing compounds
    • 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
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
    • C08K5/098—Metal salts of carboxylic acids
    • 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
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/10—Esters; Ether-esters
    • C08K5/12—Esters; Ether-esters of cyclic polycarboxylic acids
    • 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
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/13—Phenols; Phenolates
    • C08K5/134—Phenols containing ester groups
    • C08K5/1345—Carboxylic esters of phenolcarboxylic acids
    • 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
    • C08K5/00—Use of organic ingredients
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/20—Carboxylic acid amides
    • 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
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/02—Fibres or whiskers
    • C08K7/04—Fibres or whiskers inorganic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/04—Homopolymers or copolymers of ethene
    • C08L23/06—Polyethene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
    • C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L27/04—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
    • C08L27/06—Homopolymers or copolymers of vinyl chloride
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L91/00—Compositions of oils, fats or waxes; Compositions of derivatives thereof
    • C08L91/06—Waxes
    • 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
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/10—Transparent films; Clear coatings; Transparent materials

Abstract

The present invention relates to a kind of dedicated low smells in floor without phenol calcium zinc stabilizer and preparation method thereof, belongs to polyvinyl-chloride use heat stabilizer technical field.The heat stabilizer is made of the raw material of following mass percent：Main stabilizer 20%-45%, plasticizer 22%-32%；Antioxidant 3%-8%；Graphene 5%-10%；Lubricant 4%-9%；Adjuvant 5%-10%.Joined hexagonal boron nitride graphene in formula of the invention, high-specific surface area makes it have enrichment, in super polyvinyl chloride product using advantageous；The dedicated low smell in floor of the invention has good thermal stability, processability and flame retardant property without phenol calcium zinc stabilizer, and heat-stable time reached similar products at home and abroad.

Description

A kind of dedicated low smell in floor is without phenol calcium zinc stabilizer and preparation method thereof
Technical field
The present invention relates to polyvinyl-chloride use heat stabilizer, in particular to a kind of dedicated low smell in floor is without phenol calcium zinc stabilizer And preparation method thereof.
Background technique
Polyvinyl chloride (PVC) plastics are one of five big general-purpose plastics, and PVC is China first, second-biggest-in-the-world synthetic resin, Have many advantages, such as that cheap, fire retardant, corrosion-resistant and transparent performance is good, electrical insulating property is good, but the disadvantage of PVC is hot steady Qualitative difference.Mainly there is a lead salts with the industrialization heat stabilizer on PVC in the world at present, mixed metal salt, organic tin, Antimony organic class, organic auxiliary heat stabilizer, terres rares.Maximum world wide production is still traditional lead system, barium system, cadmium system class stabilization Agent.But such toxic heavy metal heat stabilizer is required constantly to mention by RoHS instruction and EUP instruction technique barrier and Chinese environmental protection High influence, occupation rate of market will constantly decline, and have the tendency that being eliminated.Calcium/zinc composite heat stabilizer due to it is nontoxic, The advantages that environmental protection, moderate cost is one of the most active field of world today's research.
Hexagonal boron nitride graphene has the characteristics such as the good transparency, high-specific surface area, Young's modulus of elasticity height, has very much Excellent properties are conducive to the raising of product mechanics mechanical performance, and can serve certain fire-retardant.But it is answered in heat stabilizer With less, therefore, it is very significant for developing a kind of dedicated low smell in floor without phenol calcium zinc stabilizer.
Summary of the invention
The purpose of the present invention is：Overcome the shortcomings of heat stabilizer when existing Corvic uses, provides a kind ofly The dedicated low smell of plate is without phenol calcium zinc stabilizer.It is steady that the present invention effectively solves the generally existing heat of present polyvinyl-chloride use heat stabilizer The problem of qualitative poor, poor fire.
Realizing the technical solution of the object of the invention is：A kind of dedicated low smell in floor is including following without phenol calcium zinc stabilizer The each component of mass percent：
The dedicated low smell in a kind of floor of the present invention preferably includes following mass percent without phenol calcium zinc stabilizer Each component：
The dedicated low smell in a kind of floor of the present invention more preferably includes following mass percent without phenol calcium zinc stabilizer Each component：
Main stabilizer described above be stearic acid, lauric acid, isooctyl acid, aphthenic acids, benzoic acid, phosphorous acid calcium salt and Two or more in zinc salt；The mass percent of the calcium salt and zinc salt is 1-8:2；And the acid group number of the calcium salt and zinc salt It is identical.
Plasticizer described above is one of di-n-octyl phthalate, diisooctyl phthalate.
Antioxidant described above is one of antioxidant 1010, antioxidant 1076, antioxidant 164, antioxidant 264.
Hexagonal boron nitride graphene described above is the grapheme material containing hexagonal boron nitride interlayer.
Lubricant described above is one of ethylene bis stearic acid amide, paraffin, polyethylene wax.
Adjuvant described above is one of magnesium stearate, aluminium hydroxide.
A kind of dedicated preparation method of the low smell without phenol calcium zinc stabilizer in floor described above, specifically includes following step Suddenly：
(1) main stabilizer for calculating proportion is added in the reaction vessel, and stirs 30-60min at 60-90 DEG C；
(2) plasticizer, lubricant, antioxidant, adjuvant are continuously added, and stirs 45-60min at 70-90 DEG C；
(3) it is eventually adding hexagonal boron nitride graphene, 20-30min is stirred at 75~95 DEG C, obtains floor after cooling Dedicated low smell is without phenol calcium zinc stabilizer.
The present invention has the effect of positive：
(1) it joined hexagonal boron nitride graphene in formula of the invention, hexagonal boron nitride graphene is in a dimension Upper maintenance nanoscale, and there is the spy of the two-dimension periodic honeycomb lattice structure of similar carbon hexatomic ring composition in two-dimensional surface Different material has many excellent properties：High-specific surface area makes it have enrichment, and adsorption capacity is big；The transparency is good, can prepare High transparency stabilizer product, in super polyvinyl chloride product using advantageous；High Young's modulus of elasticity, has Conducive to the raising of product mechanics mechanical performance.And hexagonal boron nitride graphene forms carbon-coating network in combustion, hinders The evolution of catabolite plays fire retardation.
(2) heat stabilizer preparation method provided by the invention is simple, and convenient for operation, the heat stabilizer of preparation has good Thermal stability, processability and flame retardant property, heat-stable time reached similar products at home and abroad.
Specific embodiment
Presently in connection with embodiment, the present invention is described in further detail.
Embodiment 1
Weigh following each component：
It is prepared as follows：
(1) calcium stearate and zinc stearate are added in the reaction vessel, and stirs 60min at 60 DEG C；
(2) di-n-octyl phthalate, ethylene bis stearic acid amide, antioxidant 1010, magnesium stearate are continuously added, and 60min is stirred at 70 DEG C；
(3) it is eventually adding hexagonal boron nitride graphene, 30min is stirred at 75 DEG C, it is dedicated low to obtain floor after cooling Smell is without phenol calcium zinc stabilizer.
Embodiment 2
Weigh following each component：
It is prepared as follows：
(1) calcium laurate and zinc stearate are added in the reaction vessel, and stirs 50min at 70 DEG C；
(2) diisooctyl phthalate, paraffin, antioxidant 1076, magnesium stearate are continuously added, and is stirred at 80 DEG C 55min；
(3) it is eventually adding hexagonal boron nitride graphene, 25min is stirred at 85 DEG C, it is dedicated low to obtain floor after cooling Smell is without phenol calcium zinc stabilizer.
Embodiment 3
Weigh following each component：
It is prepared as follows：
(1) calcium iso-octoate and zinc phosphite are added in the reaction vessel, and stirs 40min at 80 DEG C；
(2) diisooctyl phthalate, polyethylene wax, antioxidant 164, aluminium hydroxide are continuously added, and at 80 DEG C Stir 55min；
(3) it is eventually adding hexagonal boron nitride graphene, 25min is stirred at 85 DEG C, it is dedicated low to obtain floor after cooling Smell is without phenol calcium zinc stabilizer.
Embodiment 4
Weigh following each component：
It is prepared as follows：
(1) calcium naphthenate and zinc benzoate are added in the reaction vessel, and stirs 30min at 90 DEG C；
(2) di-n-octyl phthalate, polyethylene wax, antioxidant 264, aluminium hydroxide are continuously added, and at 90 DEG C Stir 45min；
(3) it is eventually adding hexagonal boron nitride graphene, 20min is stirred at 95 DEG C, it is dedicated low to obtain floor after cooling Smell is without phenol calcium zinc stabilizer.
Comparative example 1 is compared with embodiment 1, the difference is that：
Comparative example 1
Weigh following each component：
It is prepared as follows：
(1) calcium stearate and zinc stearate are added in the reaction vessel, and stirs 60min at 60 DEG C；
(2) di-n-octyl phthalate, ethylene bis stearic acid amide, antioxidant 1010, magnesium stearate are continuously added, and 60min is stirred at 70 DEG C, obtains the dedicated low smell in floor without phenol calcium zinc stabilizer after cooling.
Comparative example 2
Other with embodiment 1, the difference is that：Calcium stearate dosage is 100g, and zinc stearate dosage is 300g.
Comparative example 3
Other with embodiment 1, the difference is that：Calcium stearate dosage is 330g, and zinc stearate dosage is 70g.
Comparative example 4
Other with embodiment 1, the difference is that：Lubricant is not added in system.
Test method is：
Congo red method：Execution standard GB/T2917-2002.PVC sheets obtained are cut into side length just less than 2mm Rectangular or cube is packed into reaction tube, height about 50mm, slight vibration, but sample should not be made to fill reality or to be sticked to test tube excessively On wall.Congored test paper is placed in two centimeters above print particle, stoppers plug.Test tube is placed in specific test requirements document temperature Under oil bath in, observe and record the time of test paper (pH=3) from red to blue, result corresponds to initial coloring.
It can be seen that by upper table data：The heat-stable time of Example formulations is above comparative example heat stabilizer, therefore has There is good thermal stability.Moreover, the oxygen index (OI) of Example formulations increased compared with comparative example heat stabilizer, illustrate to have certain Fire retardation.
Taking the above-mentioned ideal embodiment according to the present invention as inspiration, through the above description, relevant staff is complete Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention Property range is not limited to the contents of the specification, it is necessary to which the technical scope thereof is determined according to the scope of the claim.

Claims (9)

1. a kind of dedicated low smell in floor is without phenol calcium zinc stabilizer, it is characterised in that：Each component including following mass percent：
Main stabilizer 20%-45%；
Plasticizer 22%-32%；
Antioxidant 3%-8%；
Hexagonal boron nitride graphene 5%-10%；
Lubricant 4%-9%；
Adjuvant 5%-10%.
2. the dedicated low smell in a kind of floor according to claim 1 is without phenol calcium zinc stabilizer, it is characterised in that：Including following The each component of mass percent：
Main stabilizer 30%-42%；
Plasticizer 25%-30%；
Antioxidant 3%-8%；
Hexagonal boron nitride graphene 6%-8%；
Lubricant 4%-9%；
Adjuvant 5%-10%.
3. the dedicated low smell in a kind of floor according to claim 1 is without phenol calcium zinc stabilizer, it is characterised in that：The master Stabilizer is two or more in the calcium salt and zinc salt of stearic acid, lauric acid, isooctyl acid, aphthenic acids, benzoic acid, phosphorous acid； The mass percent of the calcium salt and zinc salt is 1-8:2；And the calcium salt is identical with the acid group number of zinc salt.
4. the dedicated low smell in a kind of floor according to claim 1 is without phenol calcium zinc stabilizer, it is characterised in that：The increasing Modeling agent is one of di-n-octyl phthalate, diisooctyl phthalate.
5. the dedicated low smell in a kind of floor according to claim 1 is without phenol calcium zinc stabilizer, it is characterised in that：Described is anti- Oxygen agent is one of antioxidant 1010, antioxidant 1076, antioxidant 164, antioxidant 264.
6. the dedicated low smell in a kind of floor according to claim 1 is without phenol calcium zinc stabilizer, it is characterised in that：Six side Boron nitride graphene is the grapheme material containing hexagonal boron nitride interlayer.
7. the dedicated low smell in a kind of floor according to claim 1 is without phenol calcium zinc stabilizer, it is characterised in that：The profit Lubrication prescription is one of ethylene bis stearic acid amide, paraffin, polyethylene wax.
8. the dedicated low smell in a kind of floor according to claim 1 is without phenol calcium zinc stabilizer, it is characterised in that：Described is auxiliary Auxiliary agent is one of magnesium stearate, aluminium hydroxide.
9. a kind of dedicated preparation side of the low smell without phenol calcium zinc stabilizer in floor as described in claim 1~8 is any Method, it is characterised in that there are following steps：
（1）The main stabilizer for calculating proportion is added in the reaction vessel, and stirs 30-60min at 60-90 DEG C；
（2）Plasticizer, lubricant, antioxidant, adjuvant are continuously added, and stirs 45-60min at 70-90 DEG C；
（3）It is eventually adding hexagonal boron nitride graphene, 20-30min is stirred at 75~95 DEG C, it is dedicated to obtain floor after cooling Low smell is without phenol calcium zinc stabilizer.
CN201810585755.0A 2018-06-08 2018-06-08 A kind of dedicated low smell in floor is without phenol calcium zinc stabilizer and preparation method thereof Pending CN108841048A (en)

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CN114230866A (en) * 2022-02-23 2022-03-25 山东三义集团股份有限公司 Preparation method of calcium-zinc stabilizer

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109439290A (en) * 2018-12-05 2019-03-08 山东恒利热载体工程技术有限公司 A kind of environmental protection organic heat carrier and preparation method thereof
CN109439290B (en) * 2018-12-05 2021-03-16 山东恒利热载体工程技术有限公司 Environment-friendly organic heat carrier and preparation method thereof
CN114230866A (en) * 2022-02-23 2022-03-25 山东三义集团股份有限公司 Preparation method of calcium-zinc stabilizer

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Application publication date: 20181120