CN107312269A - A kind of composite thermal stabilizer and preparation method thereof - Google Patents
A kind of composite thermal stabilizer and preparation method thereof Download PDFInfo
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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
- 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
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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
- C08K2003/2206—Oxides; Hydroxides of metals of calcium, strontium or barium
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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
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The present invention relates to stabilizer, concretely it is a kind of composite thermal stabilizer and preparation method thereof, a kind of composite thermal stabilizer, 20 60 parts of stearic acid, 5 25 parts of calcium hydroxide, 5 25 parts of zinc oxide, 3 28 parts of pentaerythrite, 15 parts of mercaptans type heat stabilizer, 1 10 parts of cyanuric acid lanthanum, 5 15 parts of paraffin, 1 10 parts of epoxidized soybean oil, 1 10 parts of diethylene glycol, 15 parts of phenolic antioxidant, 0.1 2 parts of catalyst.The composite thermal stabilizer of the present invention has excellent heat endurance performance, i.e., with lasting heat endurance, compared to general calcium zinc stabilizer, have more preferable lubricity in PVC, and this causes there is preferable processing characteristics in PVC product.
Description
Technical field
Concretely it is a kind of composite thermal stabilizer and preparation method thereof the present invention relates to stabilizer.
Background technology
Stabilizer for plastics various types, but single composition often stability, form and aspect at initial stage, coloring, soffening, with
PVC processing requests can not be met in terms of PVC compatibility.Calcium zinc stabilizer is main flow stabilizer product in the market, main
It is calcium-zinc composite stabilizing agent to want product form, but calcium zinc stabilizer is still defective in performance, is mainly reflected in easily appearance and " burns
Zinc ", though processing color and luster at initial stage is good, occurs after " burning zinc ", accelerates the aging of product on the contrary, the lasting stability of product is poor, separately
On the one hand the product quality variance of each manufacturing enterprise is larger, and some enterprises are in order to reduce the fillers such as cost addition calcium powder, in PVC bases
Plinth is that often high pressure, phenomenon of rupture occur, and rubber and plastic processing enterprise is difficult to accept or reject on production cost and properties of product, is still using lead
Salt stabilizing agent.Calcium zinc stabilizer is only used for ordinary plastic articles, the water pipe higher for environmental requirement, ornament materials, transparent
Rely on imported product more stabilizer needed for product, high-grade plastic products, or coordinate auxiliary using the higher organic tin stabilizer of price
Co-stabilizer.
The content of the invention
The problem of present invention is for current composite thermal stabilizer lasting stability difference, the invention provides a kind of compound thermal is steady
Agent is determined, to expect to solve the above problems.
The present invention solves above-mentioned technical problem, and the technical scheme of use is, a kind of composite thermal stabilizer, including following weight
The component of number：20-60 parts of stearic acid, 5-25 parts of calcium hydroxide, 5-25 parts of zinc oxide, 3-28 parts of pentaerythrite, mercaptans type 1-5
Part, 1-10 parts of cyanuric acid lanthanum, 5-15 parts of paraffin, 1-10 parts of epoxidized soybean oil, 1-10 parts of diethylene glycol, 1-5 parts of phenolic antioxidant,
0.1-2 parts of catalyst.
A kind of composite thermal stabilizer preparation method, this method uses the component of above-mentioned composite thermal stabilizer：
(1) auxiliary agent is pre-prepared, by epoxidized soybean oil, diethylene glycol, pentaerythrite, phenolic antioxidant, paraffin in reactor
In be heated to 80-90 DEG C, stir and simultaneously obtain A materials to complete thawing；
(2) whole stearic acid are added in reactor, are heated to melting complete, during which visual Flow of Goods and Materials situation opens low speed
Stirring is to accelerate dissolution velocity, after stearic acid melts completely, and point three echelons add calcium hydroxide, zinc oxide mix to reactor
In, while catalyst is added dropwise, and high-speed stirred is opened, stir 25-45min and be heated to 100-110 DEG C, the B things melted
Material；
Wherein, above-mentioned stirring at low speed is adjusted by 0-300r/min, and above-mentioned high-speed stirred presses 600-1200r/min；Wherein
One echelon adds calcium hydroxide, the amount of zinc oxide mix is addition calcium hydroxide, the 10- of zinc oxide mix quality altogether
20%, the second echelon adds calcium hydroxide, the amount of zinc oxide mix is addition calcium hydroxide, zinc oxide mix quality altogether
10-40%, the 3rd echelon adds remaining calcium hydroxide, zinc oxide mix；
(3) cyanuric acid lanthanum, mercaptans type are added in the B materials of melting, stirred under 600-900r/min rotating speeds
Obtain C materials；
(4) A materials are added in C materials, stirring at low speed 10-20min obtains D materials；
(5) powdery composite thermal stabilizer is made by tower cooler of dusting in D materials, then obtains above-mentioned compound through extruder grain
Heat stabilizer.
Particularly, the preparation method of above-mentioned mercaptans type is：
A, a certain amount of mercaptan carboxylic acid of preparation, fatty alcohol, catalyst and appropriate organic solvent, are heated to reflux being esterified
Reaction, untill reaction water is separated completely, obtains E materials；
B, while hot the addition antimony oxide solution into E materials, continue to be heated to reflux carrying out synthetic reaction, after reaction completely
Stop heating, stand split-phase and separate aqueous phase therein while hot, organic phase is evaporated in vacuo, steam dry through vacuum after solvent
It is dry, mercapto-carboxylic ester antimony heat stabilizer is obtained, above-mentioned mercaptans type is produced.
Particularly, above-mentioned mercaptan carboxylic acid, fatty alcohol mol ratio are 1:1-1:1.2.
Particularly, in a steps, it is above-mentioned be heated to reflux carry out esterification in heating-up temperature be 80-120 DEG C.
Particularly, the preparation method of above-mentioned mercaptans type is：
C, a certain amount of mercapto-carboxylic ester of preparation, catalyst and appropriate organic solvent, heating obtain F materials；
D, while hot the addition antimony oxide solution into F materials, insulation backflow carry out synthetic reaction, stop after reaction is complete
Stirring and heating, static split-phase simultaneously separate aqueous phase, organic phase are evaporated in vacuo, steamed after solvent through being dried in vacuo while hot
To mercapto-carboxylic ester antimony, above-mentioned mercaptans type is produced.
Particularly, in step c, above-mentioned heating-up temperature is 95-120 DEG C.
Particularly, in Step d, above-mentioned insulation backflow flows back that is, at 96-100 DEG C of keeping temperature.
Particularly, above-mentioned catalyst is one or more of a variety of in P-TOLUENE SULFO ACID 99, glacial acetic acid, the concentrated sulfuric acid or concentrated hydrochloric acid
Mixture.
Particularly, above-mentioned organic solvent is in styrene, perchloroethylene, ethylene glycol ether, toluene and dimethylbenzene
One or more of a variety of mixtures.
The present invention at least has the following effects that：
The composite thermal stabilizer of the present invention has excellent heat endurance performance, i.e., with lasting heat endurance, compare
In general calcium zinc stabilizer, there is more preferable lubricity in PVC, this causes there is preferable processing characteristics in PVC product.
Embodiment
In order that the objects, technical solutions and advantages of the present invention can become apparent from understanding, with reference to embodiments to this
Invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, not
For limiting present invention protection content.
A kind of composite thermal stabilizer of the present invention, wraps the component of following parts by weight：Include the component of following parts by weight：
20-60 parts of stearic acid, 5-25 parts of calcium hydroxide, 5-25 parts of zinc oxide, 3-28 parts of pentaerythrite, 1-5 parts of mercaptans type, cyanuric acid lanthanum
1-10 parts, 5-15 parts of paraffin, 1-10 parts of epoxidized soybean oil, 1-10 parts of diethylene glycol, 1-5 parts of phenolic antioxidant, catalyst 0.1-2
Part.The content of each component number determine the composite thermal stabilizer thermal stability of the present invention, it is excessive all to cause on a small quantity
The thermal stability of this composite thermal stabilizer is not good.
Embodiment one：
A kind of composite thermal stabilizer, wraps the component of following parts by weight：55 parts of stearic acid, 4 parts of hydrogen calcium hydroxide, zinc oxide
3 parts, 5 parts of pentaerythrite, 2 parts of mercaptans type, 8 parts of cyanuric acid lanthanum, 15 parts of paraffin, 8 parts of epoxidized soybean oil, 5 parts of diethylene glycol, phenols
1 part of antioxidant, 0.1 part of catalyst.
A kind of composite thermal stabilizer preparation method, this method uses the component of above-mentioned composite thermal stabilizer：
(1) auxiliary agent is pre-prepared, by epoxidized soybean oil, diethylene glycol, pentaerythrite, phenolic antioxidant, paraffin in reactor
In be heated to 85 DEG C, stir and simultaneously obtain A materials to complete thawing；
(2) whole stearic acid are added in reactor, are heated to melting complete, during which visual Flow of Goods and Materials situation opens low speed
Stirring is to accelerate dissolution velocity, after stearic acid melts completely, and point three echelons add calcium hydroxide, zinc oxide mix to reactor
In, while catalyst is added dropwise, and high-speed stirred is opened, stir 30min and be heated to 105 DEG C, the B materials melted；
Wherein, above-mentioned stirring at low speed is adjusted by 0-300r/min, and above-mentioned high-speed stirred presses 1100r/min；Wherein first ladder
Secondary addition calcium hydroxide, the amount of zinc oxide mix are addition calcium hydroxide, the 20% of zinc oxide mix quality, second altogether
Echelon adds the amount of calcium hydroxide, zinc oxide mix to add calcium hydroxide, the 30% of zinc oxide mix quality altogether, the
Three echelons add remaining calcium hydroxide, zinc oxide mix；
(3) cyanuric acid lanthanum, mercaptans type are added in the B materials of melting, C is uniformly mixing to obtain under 700r/min rotating speeds
Material；
(4) A materials are added in C materials, stirring at low speed 15min obtains D materials；
(5) powdery composite thermal stabilizer is made by tower cooler of dusting in D materials, then obtains above-mentioned compound through extruder grain
Heat stabilizer.
The composite thermal stabilizer of the present embodiment has excellent heat endurance performance, i.e., with lasting heat endurance, phase
Than in general calcium zinc stabilizer, having more preferable lubricity in PVC, this causes there is preferable processability in PVC product
Energy.
Embodiment two：
A kind of composite thermal stabilizer, wraps the component of following parts by weight：60 parts of stearic acid, 10 parts of hydrogen calcium hydroxide, oxidation
8 parts of zinc, 10 parts of pentaerythrite, 2 parts of mercaptans type, 5 parts of cyanuric acid lanthanum, 15 parts of paraffin, 5 parts of epoxidized soybean oil, 5 parts of diethylene glycol,
5 parts of phenolic antioxidant, 2 parts of catalyst.
A kind of composite thermal stabilizer preparation method, this method uses the component of above-mentioned composite thermal stabilizer：
(1) auxiliary agent is pre-prepared, by epoxidized soybean oil, diethylene glycol, pentaerythrite, phenolic antioxidant, paraffin in reactor
In be heated to 80 DEG C, stir and simultaneously obtain A materials to complete thawing；
(2) whole stearic acid are added in reactor, are heated to melting complete, during which visual Flow of Goods and Materials situation opens low speed
Stirring is to accelerate dissolution velocity, after stearic acid melts completely, and point three echelons add calcium hydroxide, zinc oxide mix to reactor
In, while catalyst is added dropwise, and high-speed stirred is opened, stir 45min and be heated to 110 DEG C, the B materials melted；
Wherein, above-mentioned stirring at low speed is adjusted by 0-300r/min, and above-mentioned high-speed stirred presses 1200r/min；Wherein first ladder
Secondary addition calcium hydroxide, the amount of zinc oxide mix are addition calcium hydroxide, the 10% of zinc oxide mix quality, second altogether
Echelon adds the amount of calcium hydroxide, zinc oxide mix to add calcium hydroxide, the 10% of zinc oxide mix quality altogether, the
Three echelons add remaining calcium hydroxide, zinc oxide mix；
(3) cyanuric acid lanthanum, mercaptans type are added in the B materials of melting, C is uniformly mixing to obtain under 900r/min rotating speeds
Material；
(4) A materials are added in C materials, stirring at low speed 10min obtains D materials；
(5) powdery composite thermal stabilizer is made by tower cooler of dusting in D materials, then obtains above-mentioned compound through extruder grain
Heat stabilizer.
Embodiment three：
A kind of composite thermal stabilizer, wraps the component of following parts by weight：20 parts of stearic acid, 6 parts of hydrogen calcium hydroxide, zinc oxide
5 parts, 3 parts of pentaerythrite, 1 part of mercaptans type, 1 part of cyanuric acid lanthanum, 5 parts of paraffin, 1 part of epoxidized soybean oil, 1 part of diethylene glycol, phenols
1 part of antioxidant, 0.1 part of catalyst.
A kind of composite thermal stabilizer preparation method, this method uses the component of above-mentioned composite thermal stabilizer：
(1) auxiliary agent is pre-prepared, by epoxidized soybean oil, diethylene glycol, pentaerythrite, phenolic antioxidant, paraffin in reactor
In be heated to 80 DEG C, stir and simultaneously obtain A materials to complete thawing；
(2) whole stearic acid are added in reactor, are heated to melting complete, during which visual Flow of Goods and Materials situation opens low speed
Stirring is to accelerate dissolution velocity, after stearic acid melts completely, and point three echelons add calcium hydroxide, zinc oxide mix to reactor
In, while catalyst is added dropwise, and high-speed stirred is opened, stir 25min and be heated to 100 DEG C, the B materials melted；
Wherein, above-mentioned stirring at low speed is adjusted by 0-300r/min, and above-mentioned high-speed stirred presses 1000r/min；Wherein first ladder
Secondary addition calcium hydroxide, the amount of zinc oxide mix are addition calcium hydroxide, the 10% of zinc oxide mix quality, second altogether
Echelon adds the amount of calcium hydroxide, zinc oxide mix to add calcium hydroxide, the 40% of zinc oxide mix quality altogether, the
Three echelons add remaining calcium hydroxide, zinc oxide mix；
(3) cyanuric acid lanthanum, mercaptans type are added in the B materials of melting, C is uniformly mixing to obtain under 600r/min rotating speeds
Material；
(4) A materials are added in C materials, stirring at low speed 20min obtains D materials；
(5) powdery composite thermal stabilizer is made by tower cooler of dusting in D materials, then obtains above-mentioned compound through extruder grain
Heat stabilizer.
The mercaptans type that the mercaptans type that above-described embodiment one is used to embodiment three is typically bought in the market.
Example IV：
On the basis of embodiment one, the preparation method of above-mentioned mercaptans type is：
C, a certain amount of mercaptan carboxylic acid of preparation, fatty alcohol, glacial acetic acid and appropriate toluene, are heated to reflux progress and are esterified instead
Should, untill reaction water is separated completely, obtain E materials；
D, while hot the addition antimony oxide solution into E materials, continue to be heated to reflux carrying out synthetic reaction, after reaction completely
Stop heating, stand split-phase and separate aqueous phase therein while hot, organic phase is evaporated in vacuo, steam dry through vacuum after solvent
It is dry, mercapto-carboxylic ester antimony heat stabilizer is obtained, above-mentioned mercaptans type is produced.
Above-mentioned mercaptan carboxylic acid, fatty alcohol mol ratio are 1:1.
In a steps, it is above-mentioned be heated to reflux carry out esterification in heating-up temperature be 80 DEG C.
Embodiment five：
From unlike example IV, above-mentioned mercaptan carboxylic acid, fatty alcohol mol ratio be 1:1.2；It is above-mentioned to add in a steps
Heat is returned
It is 120 DEG C that stream, which carries out heating-up temperature in esterification,.
Embodiment six：
On the basis of embodiment one, the preparation method of above-mentioned mercaptans type is：
C, a certain amount of mercapto-carboxylic ester of preparation, the concentrated sulfuric acid and appropriate styrene, heating obtain F materials；
D, while hot the addition antimony oxide solution into F materials, insulation backflow carry out synthetic reaction, stop after reaction is complete
Stirring and heating, static split-phase simultaneously separate aqueous phase, organic phase are evaporated in vacuo, steamed after solvent through being dried in vacuo while hot
To mercapto-carboxylic ester antimony, above-mentioned mercaptans type is produced.
In step c, above-mentioned heating-up temperature is 95 DEG C.
In Step d, above-mentioned insulation backflow flows back that is, at 96 DEG C of keeping temperature.
Embodiment seven：
On the basis of embodiment one, the preparation method of above-mentioned mercaptans type is：
C, a certain amount of mercapto-carboxylic ester of preparation, P-TOLUENE SULFO ACID 99 and appropriate organic solvent, heating obtain F materials；
D, while hot the addition antimony oxide solution into F materials, insulation backflow carry out synthetic reaction, stop after reaction is complete
Stirring and heating, static split-phase simultaneously separate aqueous phase, organic phase are evaporated in vacuo, steamed after solvent through being dried in vacuo while hot
To mercapto-carboxylic ester antimony, above-mentioned mercaptans type is produced.
In step c, above-mentioned heating-up temperature is 120 DEG C.
In Step d, above-mentioned insulation backflow flows back that is, at 100 DEG C of keeping temperature.
According to the mass fraction, the hot composite thermal stabilizer ratio for taking PVC to be obtained with above-described embodiment one to seven：50:1 mixing,
It is uniformly mixing to obtain PVC test materials.
The test material obtained to above-described embodiment is tested：
Static heat stability is tested：GB/T2917-2002；The test of RM-200A torque rheometers (survey by dynamic thermal stability
Examination), 200 DEG C of temperature, rotating speed 30r/min；Electronic universal tester tensile property is tested：GB/T1041-2006,5mm/min；It is outstanding
Arm beam shock machine impact strength is tested：GB/T1843-1996.
| Performance | Embodiment one | Embodiment two | Embodiment three |
| Static heat-stable time (min) | 156 | 141 | 145 |
| Dynamic heat-stable time (min) | 53.2 | 40.9 | 43.3 |
| Plastify moment of torsion (Nm) | 46.1 | 38.5 | 42.0 |
| Counter balance torque (Nm) | 39.4 | 36.9 | 39.2 |
| Counter balance torque temperature (DEG C) | 207.3 | 209.1 | 207.6 |
| Tensile strength (MPa) | 45.2 | 45.8 | 46.7 |
| Impact strength (kjm2) | 8.5 | 8.2 | 8.8 |
| Performance | Example IV | Embodiment five | Embodiment six | Embodiment seven |
| Static heat-stable time (min) | 153 | 151 | 148 | 146 |
| Dynamic heat-stable time (min) | 47.5 | 43.4 | 45.1 | 43.8 |
| Plastify moment of torsion (Nm) | 47.9 | 46.6 | 44.1 | 41.6 |
| Counter balance torque (Nm) | 42.0 | 41.2 | 42.4 | 39.9 |
| Counter balance torque temperature (DEG C) | 208.4 | 210.4 | 209.5 | 208.7 |
| Tensile strength (MPa) | 48.3 | 49.8 | 48.5 | 47.9 |
| Impact strength (kjm2) | 8.8 | 9.0 | 8.5 | 8.2 |
Claims (10)
1. a kind of composite thermal stabilizer, it is characterised in that：Include the component of following parts by weight：20-60 parts of stearic acid, hydroxide
5-25 parts of calcium, 5-25 parts of zinc oxide, 3-28 parts of pentaerythrite, 1-5 parts of mercaptans type heat stabilizer, 1-10 parts of cyanuric acid lanthanum, paraffin
5-15 parts, 1-10 parts of epoxidized soybean oil, 1-10 parts of diethylene glycol, 1-5 parts of phenolic antioxidant, 0.1-2 parts of catalyst.
2. a kind of composite thermal stabilizer preparation method, it is characterised in that：Described method is steady using compound thermal described in claim 1
Determine the component of agent, comprise the following steps：
(1) auxiliary agent is pre-prepared, and epoxidized soybean oil, diethylene glycol, pentaerythrite, phenolic antioxidant, paraffin are added in a kettle.
Heat stirs to 80-90 DEG C and obtains A materials to melting completely；
(2) whole stearic acid are added in reactor, are heated to melting complete, during which visual Flow of Goods and Materials situation opens stirring at low speed
To accelerate dissolution velocity, after stearic acid melts completely, point three echelons add calcium hydroxide, zinc oxide mix into reactor,
Catalyst is added dropwise simultaneously, and opens high-speed stirred, stirs 25-45min and is heated to 100-110 DEG C, the B materials melted；
Wherein, the stirring at low speed is adjusted by 0-300r/min, and the high-speed stirred presses 600-1200r/min；Wherein first ladder
Secondary addition calcium hydroxide, the amount of zinc oxide mix are to add calcium hydroxide, the 10-20% of zinc oxide mix quality altogether,
Second echelon adds calcium hydroxide, the amount of zinc oxide mix is addition calcium hydroxide, the 10- of zinc oxide mix quality altogether
40%, the 3rd echelon adds remaining calcium hydroxide, zinc oxide mix；
(3) cyanuric acid lanthanum, mercaptans type heat stabilizer are added in the B materials of melting, stirred under 600-900r/min rotating speeds
Uniformly obtain C materials；
(4) A materials are added in C materials, stirring at low speed 10-20min obtains D materials；
(5) powdery composite thermal stabilizer is made by tower cooler of dusting in D materials, then through extruder grain to obtain the compound thermal steady
Determine agent.
3. a kind of composite thermal stabilizer preparation method according to claim 2, it is characterised in that：The mercaptans type is thermally-stabilised
The preparation method of agent is：
A, a certain amount of mercaptan carboxylic acid of preparation, fatty alcohol, catalyst and appropriate organic solvent, are heated to reflux progress and are esterified instead
Should, untill reaction water is separated completely, obtain E materials；
B, while hot the addition antimony oxide solution into E materials, continue to be heated to reflux carrying out stopping after synthetic reaction, reaction completely
Heating, stands split-phase and separates aqueous phase therein while hot, organic phase is evaporated in vacuo, and steams through vacuum drying after solvent,
Mercapto-carboxylic ester antimony heat stabilizer is obtained, mercaptans type heat stabilizer is produced.
4. a kind of composite thermal stabilizer preparation method according to claim 3, it is characterised in that：The mercaptan carboxylic acid, fat
Fat alcohol mol ratio is 1:1-1:1.2.
5. a kind of composite thermal stabilizer preparation method according to claim 3, it is characterised in that：It is described to add in a steps
It is 80-120 DEG C that heat backflow, which carries out heating-up temperature in esterification,.
6. a kind of composite thermal stabilizer preparation method according to claim 2, it is characterised in that：The mercaptans type is thermally-stabilised
The preparation method of agent is：
C, a certain amount of mercapto-carboxylic ester of preparation, catalyst and appropriate organic solvent, heating obtain F materials；
D, while hot the addition antimony oxide solution into F materials, insulation backflow carry out synthetic reaction, and stirring is stopped after reaction is complete
And heating, static split-phase simultaneously separates aqueous phase, organic phase is evaporated in vacuo while hot, steams after solvent and to obtain mercapto through vacuum drying
Yl carboxylic acid ester antimony, produces mercaptans type heat stabilizer.
7. a kind of composite thermal stabilizer preparation method according to claim 6, it is characterised in that：It is described to add in step c
Hot temperature is 95-120 DEG C.
8. a kind of composite thermal stabilizer preparation method according to claim 6, it is characterised in that：It is described to protect in Step d
Temperature backflow, i.e., flow back at 96-100 DEG C of keeping temperature.
9. a kind of composite thermal stabilizer preparation method described in any one according to claim 3-6, it is characterised in that：
The catalyst is one or more of a variety of mixtures in P-TOLUENE SULFO ACID 99, glacial acetic acid, the concentrated sulfuric acid or concentrated hydrochloric acid.
10. a kind of composite thermal stabilizer preparation method described in any one according to claim 3-6, its feature exists
In：The organic solvent is one or more of a variety of in styrene, perchloroethylene, ethylene glycol ether, toluene and dimethylbenzene
Mixture.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113929966A (en) * | 2021-10-27 | 2022-01-14 | 浙江知友塑料科技有限公司 | Formula and production process of high-stability liquid calcium-zinc stabilizer |
| CN115505170A (en) * | 2022-10-11 | 2022-12-23 | 青岛厚德天圆创新科技有限公司 | Zinc burning inhibitor and preparation method thereof |
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| CN103435943A (en) * | 2013-09-10 | 2013-12-11 | 天津道俊包装制品销售有限公司 | Novel lanthanum cyanurate composite PVC (polyvinyl chloride) heat stabilizer |
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| CN113929966A (en) * | 2021-10-27 | 2022-01-14 | 浙江知友塑料科技有限公司 | Formula and production process of high-stability liquid calcium-zinc stabilizer |
| CN115505170A (en) * | 2022-10-11 | 2022-12-23 | 青岛厚德天圆创新科技有限公司 | Zinc burning inhibitor and preparation method thereof |
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Application publication date: 20171103 |