CN112457522A - Environment-friendly efficient dust-free composite heat stabilizer and preparation method thereof - Google Patents
Environment-friendly efficient dust-free composite heat stabilizer and preparation method thereof Download PDFInfo
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- CN112457522A CN112457522A CN202011509900.0A CN202011509900A CN112457522A CN 112457522 A CN112457522 A CN 112457522A CN 202011509900 A CN202011509900 A CN 202011509900A CN 112457522 A CN112457522 A CN 112457522A
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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
- 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
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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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
- C08K5/053—Polyhydroxylic alcohols
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- 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
- C08K5/138—Phenolates
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- 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
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
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- 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
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- 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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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Abstract
The invention discloses an environment-friendly high-efficiency dust-free composite heat stabilizer and a preparation method thereof, wherein the dust-free composite heat stabilizer is prepared from the following raw materials in parts by weight: 40-60 parts of salicylic acid rare earth stabilizer, 14-28 parts of calcium stearate, 5-8 parts of beta-diketone, 6-12 parts of polyol, 4-8 parts of phosphite ester and 2-6 parts of lubricant. The environment-friendly efficient dust-free composite heat stabilizer provided by the invention is non-toxic and pollution-free, endows PVC products with good stable plasticizing performance, processing performance and mechanical property, has excellent heat resistance, light resistance and weather resistance, and has good plasticizing and coupling effects; the components of the composite heat stabilizer are compounded into the composite stabilizer in a molten state, so that the dust pollution is reduced, the operation is simple, and the implementation is easy; the composite heat stabilizer solves the problems of poor initial colorability, short heat stabilization time and weak weather resistance of a single rare earth heat stabilizer, has obvious synergistic effect with other heat stabilizers, and obviously improves the stability of the compounded rare earth heat stabilizer.
Description
Technical Field
The invention belongs to the technical field of PVC (polyvinyl chloride) heat stabilizers, and particularly relates to an environment-friendly efficient dust-free composite heat stabilizer and a preparation method thereof.
Technical Field
Polyvinyl chloride (PVC) is a multipurpose plastic and can be processed using various technologies, which are applied throughout various fields of the national economy, but PVC is easily thermally degraded during processing to generate hydrogen chloride, and hydrogen chloride has a catalytic and accelerated degradation effect. Therefore, it is often necessary to add thermal stabilizers to inhibit thermal degradation and improve the performance of PVC articles.
The commonly used heat stabilizers include lead salts, metals, liquid composite stabilizers, phosphorous acid and vinegar, and organotins. Wherein the lead salt heat stabilizer has good long-term heat stability, low price and toxicity; the organic tin heat stabilizer has good heat stability, but is expensive; the metal soap heat stabilizer has the advantages that the lead soap and the cadmium soap are good in stability but toxic, the calcium soap and the barium soap are poor in initial thermal stability, the zinc soap is good in initial thermal stability but poor in durability, and the phenomenon of zinc burning is easy to occur. The stabilizers used in developed countries in the world at present tend to adopt nontoxic high-efficiency composite stabilizers. The invention patent CN101440174A discloses a calcium-zinc composite heat stabilizer with excellent thermal stability, which is prepared by mixing calcium soap, high molecular zinc soap, polyol and antioxidant according to a certain proportion at normal temperature and normal pressure, and has the characteristics of good thermal stability and anti-coloring property for chlorine-containing resin, no toxicity, no heavy metal pollution and the like. However, the preparation process of the high molecular zinc soap is complicated, thereby increasing the cost of the whole composite stabilizer.
The rare earth resources in China are rich, the abundance is high, the exploitation is easy, and the proven reserves account for about 80% of the worldwide proven reserves, so the development of rare earth products in China has favorable conditions. The rare earth heat stabilizer is a newly developed heat stabilizer, has the characteristics of no toxicity, no pollution, multiple functions and the like, and has very excellent and unique performance on the heat stability of PVC. Therefore, the development of the rare earth heat stabilizer with low price and high performance has very important significance.
Disclosure of Invention
Aiming at the defects that the lead-cadmium composite heat stabilizer in the prior art is serious in toxic pollution, the zinc composite heat stabilizer is easy to generate a zinc burning phenomenon, the organic tin composite heat stabilizer is high in cost, large in peculiar smell and the like, the invention provides the environment-friendly, efficient and dust-free rare earth composite heat stabilizer which has the advantages of no toxicity, no dust, good heat stability and good weather resistance.
In order to realize the purpose of the invention, the invention is realized by adopting the following technical scheme:
an environment-friendly efficient dust-free composite heat stabilizer and a preparation method thereof are characterized by being prepared from the following raw materials in parts by weight:
40-60 parts of salicylic acid rare earth stabilizer, 14-28 parts of calcium stearate, 5-8 parts of beta-diketone, 6-12 parts of polyol, 4-8 parts of phosphite ester and 2-6 parts of lubricant.
Preferably, the environment-friendly efficient dust-free composite heat stabilizer and the preparation method thereof are characterized by being prepared from the following raw materials in parts by weight:
45 parts of salicylic acid rare earth stabilizer, 20 parts of calcium stearate, 6 parts of beta-diketone, 10 parts of polyol, 6 parts of phosphite ester and 4 parts of lubricant.
Preferably, the rare earth element in the salicylic acid rare earth stabilizer at least comprises one of lanthanum, cerium, praseodymium, neodymium, samarium and yttrium.
Preferably, the polyhydric alcohol includes at least one of 1, 4-butanediol, 1, 3-butanediol, glycerol, cyclohexanol, and pentaerythritol.
Further preferably, the polyol is pentaerythritol.
Preferably, the lubricant is at least one of paraffin wax, PE wax, oxidized polyethylene wax and monoglyceride.
The preparation method comprises the following steps: mixing the salicylic acid rare earth stabilizer, calcium stearate and beta-diketone, heating to 80-105 ℃, stirring and refluxing for 10-30 min, then sequentially adding phosphite ester, polyol and lubricant, heating to 100-125 ℃, stirring and refluxing for 15-40 min, and cooling to room temperature to obtain the environment-friendly high-efficiency dust-free composite heat stabilizer.
The invention has the beneficial effects that: 1. the environment-friendly efficient dust-free composite heat stabilizer provided by the invention is non-toxic and pollution-free, endows PVC products with good stable plasticizing performance, processing performance and mechanical property, has excellent heat resistance, light resistance and weather resistance, and has good plasticizing and coupling effects; 2. the components of the composite heat stabilizer are compounded into the composite stabilizer in a molten state, so that dust pollution is reduced, and the composite heat stabilizer is simple to operate and easy to implement; 3. the composite heat stabilizer solves the problems of poor initial colorability, short heat stabilization time and weak weather resistance of a single rare earth heat stabilizer, has obvious synergistic effect with other heat stabilizers, and remarkably improves the stability of the compounded rare earth heat stabilizer.
Detailed Description
The present invention will be further described with reference to specific examples so that those skilled in the art may better understand the present invention, but the present invention is not limited thereto.
Example 1:
an environment-friendly efficient dust-free composite heat stabilizer and a preparation method thereof are characterized by being prepared from the following raw materials in parts by weight: 45 parts of lanthanum salicylate heat stabilizer, 20 parts of calcium stearate, 6 parts of beta-diketone, 10 parts of pentaerythritol, 6 parts of phosphite ester and 4 parts of PE wax.
The preparation method comprises the following steps: mixing the lanthanum salicylate heat stabilizer, calcium stearate and beta-diketone, heating to 80-105 ℃, stirring and refluxing for 10-30 min, then sequentially adding phosphite ester, pentaerythritol and PE wax, heating to 100-125 ℃, stirring and refluxing for 15-40 min, and then cooling to room temperature to obtain the environment-friendly high-efficiency dust-free composite heat stabilizer.
Example 2:
an environment-friendly efficient dust-free composite heat stabilizer and a preparation method thereof are characterized by being prepared from the following raw materials in parts by weight: 40 parts of lanthanum salicylate heat stabilizer, 18 parts of calcium stearate, 8 parts of beta-diketone, 6 parts of pentaerythritol, 4 parts of phosphite ester and 2 parts of PE wax.
The preparation method comprises the following steps: mixing the lanthanum salicylate heat stabilizer, calcium stearate and beta-diketone, heating to 80-105 ℃, stirring and refluxing for 10-30 min, then sequentially adding phosphite ester, pentaerythritol and PE wax, heating to 100-125 ℃, stirring and refluxing for 15-40 min, and then cooling to room temperature to obtain the environment-friendly high-efficiency dust-free composite heat stabilizer.
Example 3:
an environment-friendly efficient dust-free composite heat stabilizer and a preparation method thereof are characterized by being prepared from the following raw materials in parts by weight: 50 parts of cerium salicylate heat stabilizer, 18 parts of calcium stearate, 6 parts of beta-diketone, 8 parts of 1, 4-butanediol, 5 parts of phosphite ester and 2 parts of PE wax.
The preparation method comprises the following steps: mixing the cerium salicylate heat stabilizer, calcium stearate and beta-diketone, heating to 80-105 ℃, stirring and refluxing for 10-30 min, then sequentially adding phosphite ester, 1, 4-butanediol and PE wax, heating to 100-125 ℃, stirring and refluxing for 15-40 min, and then cooling to room temperature to obtain the environment-friendly efficient dust-free composite heat stabilizer.
Example 4:
an environment-friendly high-efficiency dust-free composite heat stabilizer and a preparation method thereof are characterized in that the environment-friendly high-efficiency dust-free composite heat stabilizer is prepared from the following raw material components in parts by weight
45 parts of a stabilizer, 20 parts of calcium stearate, 8 parts of beta-diketone, 6 parts of 1, 4-butanediol, 5 parts of phosphite ester and 2 parts of PE wax.
The preparation method comprises the following steps: mixing the cerium salicylate heat stabilizer, calcium stearate and beta-diketone, heating to 80-105 ℃, stirring and refluxing for 10-30 min, then sequentially adding phosphite ester, 1, 4-butanediol and PE wax, heating to 100-125 ℃, stirring and refluxing for 15-40 min, and then cooling to room temperature to obtain the environment-friendly efficient dust-free composite heat stabilizer.
Comparative example 1:
an environment-friendly efficient dust-free composite heat stabilizer and a preparation method thereof are characterized by being prepared from the following raw materials in parts by weight: 45 parts of lanthanum salicylate heat stabilizer, 10 parts of pentaerythritol, 6 parts of phosphite ester and 4 parts of PE wax.
The preparation method comprises the following steps: heating the lanthanum salicylate heat stabilizer to 80-105 ℃, stirring and refluxing for 10-30 min, then sequentially adding phosphite ester, pentaerythritol and PE wax, heating to 100-125 ℃, stirring and refluxing for 15-40 min, and then cooling to room temperature to obtain the environment-friendly high-efficiency dust-free composite heat stabilizer.
Comparative example 2:
an environment-friendly efficient dust-free composite heat stabilizer and a preparation method thereof are characterized by being prepared from the following raw materials in parts by weight: 50 parts of cerium salicylate heat stabilizer, 8 parts of 1, 4-butanediol, 5 parts of phosphite ester and 2 parts of PE wax.
The preparation method comprises the following steps: heating the cerium salicylate heat stabilizer to 80-105 ℃, stirring and refluxing for 10-30 min, then sequentially adding phosphite ester, 1, 4-butanediol and PE wax, heating to 100-125 ℃, stirring and refluxing for 15-40 min, and then cooling to room temperature to obtain the environment-friendly high-efficiency dust-free composite heat stabilizer.
Experimental example 1: static thermal stability test
The composite heat stabilizer prepared in examples 1-4 and the composite heat stabilizer (4 parts) prepared in comparative examples 1-2 are respectively and uniformly mixed with DOP (50 parts) and PVC (100 parts), and are plasticated for 3min on a double-roller machine with the roller temperature of 160 ℃ and the roller spacing of 1mm to prepare PVC materials 1-6. The static thermal stability of the composite is determined according to the national standard GB/T2917.1-2002 Congo red method, and the test results are shown in Table 1.
TABLE 1 static thermal stability test results
| Sample (I) | Static thermal stability time/min | |
| Example 1 | PVC Material 1 | 112.5 |
| Example 2 | PVC Material 2 | 110.9 |
| Example 3 | PVC Material 3 | 111.6 |
| Example 4 | PVC Material 4 | 108.6 |
| Comparative example 1 | PVC Material 5 | 63.2 |
| Comparative example 2 | PVC Material 6 | 54.2 |
As can be seen from the experimental data in Table 1, compared with a single rare earth heat stabilizer, the composite heat stabilizer can obviously improve the heat stability of PVC and has excellent long-term heat stability.
Experimental example 2: dynamic machining experiment
The composite heat stabilizers prepared in examples 1 to 4 and the composite heat stabilizers (4 parts) prepared in comparative examples 1 to 2 were respectively and uniformly mixed with DOP (50 parts) and PVC (100 parts), plasticated for 5min on a two-roll plasticator with a roll temperature of 180 ℃ and a roll gap of 1mm, sheeted on a flat vulcanizing machine, cut into dumbbell shapes on a universal sampling machine, and tested according to the standards, with the test results shown in Table 2.
TABLE 2 Effect of composite Heat stabilizer on PVC processability
| Plastification time/min | Equilibrium torque/Nm | Impact Strength/KJ.m-2 | Elongation at Break/Nm | |
| Pure PVC | 1.2 | 10.8 | 60 | 110 |
| Example 1 | 7.6 | 24.6 | 69 | 124 |
| Example 2 | 7.3 | 23.8 | 67 | 118 |
| Example 3 | 7.4 | 24.1 | 68 | 120 |
| Example 4 | 7.1 | 23.6 | 65 | 116 |
| Comparative example 1 | 4.2 | 15.8 | 63 | 117 |
| Comparative example 2 | 3.8 | 12.5 | 61 | 115 |
As can be seen from the experimental data in Table 2, the composite heat stabilizer can obviously promote plasticization, reduce equilibrium torque and has excellent dynamic processing performance.
Claims (5)
1. An environment-friendly efficient dust-free composite heat stabilizer is characterized by being prepared from the following raw materials in parts by weight:
40-60 parts of salicylic acid rare earth stabilizer, 14-28 parts of calcium stearate, 5-8 parts of beta-diketone, 6-12 parts of polyol, 4-8 parts of phosphite ester and 2-6 parts of lubricant.
2. The environment-friendly efficient dust-free composite heat stabilizer according to claim 1, which is prepared from the following raw materials in parts by weight:
45 parts of salicylic acid rare earth stabilizer, 20 parts of calcium stearate, 6 parts of beta-diketone, 10 parts of polyol, 6 parts of phosphite ester and 4 parts of lubricant.
3. The environment-friendly efficient dust-free composite heat stabilizer according to claim 1, wherein the rare earth element in the salicylic acid rare earth stabilizer comprises at least one of lanthanum, cerium, praseodymium, neodymium, samarium and yttrium.
4. The environment-friendly high-efficiency dust-free composite heat stabilizer according to claim 1, wherein the polyol comprises at least one of 1, 4-butanediol, 1, 3-butanediol, glycerol, cyclohexanol and pentaerythritol.
5. The environment-friendly efficient dust-free composite heat stabilizer according to claim 1, which is prepared by the following steps: mixing the salicylic acid rare earth stabilizer, calcium stearate and beta-diketone, heating to 80-105 ℃, stirring and refluxing for 10-30 min, then sequentially adding phosphite ester, polyol and lubricant, heating to 100-125 ℃, stirring and refluxing for 15-40 min, and cooling to room temperature to obtain the environment-friendly high-efficiency dust-free composite heat stabilizer.
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Citations (6)
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| CN102942712A (en) * | 2012-10-12 | 2013-02-27 | 福建师范大学 | Preparation method of luminescence composite heat stabilizer |
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| CN107082974A (en) * | 2017-04-24 | 2017-08-22 | 内蒙古科技大学 | Rare earth composite PVC heat stabilizer and preparation method thereof |
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2020
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| US20130317157A1 (en) * | 2011-02-16 | 2013-11-28 | Adeka Corporation | Vinyl chloride resin composition |
| CN102942712A (en) * | 2012-10-12 | 2013-02-27 | 福建师范大学 | Preparation method of luminescence composite heat stabilizer |
| CN105801908A (en) * | 2016-04-18 | 2016-07-27 | 广州煌垅生物科技有限公司 | Composite heat stabilizer and preparing method thereof |
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| CN107474446A (en) * | 2017-10-16 | 2017-12-15 | 天津城建大学 | A kind of liquid-type nano rare earth complex compound composite thermal stabilizer |
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Application publication date: 20210309 |