CN105273223B - Hydroxo complex heat stabilizer, composite thermal stabilizer and poly (vinyl chloride) resin composition and preparation method - Google Patents
Hydroxo complex heat stabilizer, composite thermal stabilizer and poly (vinyl chloride) resin composition and preparation method Download PDFInfo
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Abstract
The present invention provides a kind of hydroxo complex heat stabilizer, composite thermal stabilizer and poly (vinyl chloride) resin composition and preparation method, and the heat stabilizer is hydroxyl calcium complex and/or hydroxyl zinc complex.The advantage of the invention is that prepared composite thermal stabilizer is used for the stabilizer of the plastic processing such as PVC, with being difficult to separate out, the characteristics of nontoxic, cheap, stablizing effect is good.
Description
Technical field
The invention belongs to polyvinyl chloride (PVC) processing aid technical field, and in particular to a kind of hydroxo complex is thermally-stabilised
Agent, polyvinyl-chloride use composite thermal stabilizer, poly (vinyl chloride) resin composition, and preparation method.
Background technology
In recent years, with the development of modern science and technology, macromolecular material is increasingly favored by people, polyvinyl chloride resin due to
Processing technology is simple, cheap, is widely used in building, agricultural and consumer goods industries.PVC maximum shortcoming is hot steady
It is fixed poor, the degradation reaction that dehydrochlorination occurs is easy at relatively low temperature (100~200 DEG C), lose hydrogen chloride at 200 DEG C
Quickly, polymer is made to become dark, intensity is very low, has had a strong impact on its application.Therefore, heat is must be added to when PVC is processed
Stabilizer.
PVC plastic heat stabilizer has gone through several generations product by the development of decades, and lead salt stabilizer is earliest
Using, heat endurance is best, production and application technology kind the most ripe, the toxicity of heavy metal lead is its fatal defects, with
Industry and the development of society, the requirement more and more higher to environment, in developed countries such as America and Europes, lead salt type thermal stabilizing agent is little
Use, the substitute is nontoxic Ca-Zn composite heat stabilizer.China is a developing country, and lead salt stabilizer still exists
Largely use, but its cause pollution environment, public hazards the problems such as caused the attention of relevant departments, PVC heat stabilizer is nontoxic
Environmental protection is also trend of the times.In recent years, the work such as the domestic research and development for also largely putting into non-toxic heat stabilizer, production and application
In, calcium/zinc composite heat stabilizer is one of most important of which kind.
The thermal stability of single calcium/zinc heat stabilizer cannot meet application requirement, and generally for improving, its is thermally-stabilised
Performance also needs to add some auxiliary heat stabilizers, mainly there is polyalcohol, beta-diketon, phosphite ester, epoxide, hydrotalcite
And zeolite.But effect is still limited so that the application field of calcium/zinc composite heat stabilizer is restricted.
CN102153824A discloses a kind of pentaerythrite using hydroxyl with the salt of zinc three of zinc salt preparation as PVC
Heat stabilizer, have the advantages that to be difficult to separate out, stablizing effect it is good, but reaction requires that temperature is too high, and tends to have crystallization and occurs, instead
Condition is answered to be difficult to control.CN10717526A discloses a kind of polyols blend, carboxylic acid and zinc salt reaction and prepares polyol ester zinc salt
Heat stabilizer, noxious material dimethylbenzene has been used in the preparation technology, and final product is not disposable, it is difficult to take out.
Although the preparation method of existing various composite thermal stabilizers, otherwise the heat stabilizer course of reaction requirement for preparing is severe
Carve, otherwise can not meet the trend of present heat stabilizer asepsis environment-protecting.
The content of the invention
For the problem that PVC heat stabilizer in the prior art is present, a kind of hydroxo complex heat stabilizer of offer of the invention,
Composite thermal stabilizer and poly (vinyl chloride) resin composition and preparation method, to improve the thermal stability of PVC, the preparation method work
Skill is simple, and reaction temperature is relatively low, it is not necessary to catalyst, and raw material is cheap and easy to get, and environment-protecting asepsis.
The first aspect of the present invention is to provide a kind of hydroxo complex heat stabilizer, and the heat stabilizer is hydroxyl calcium complex
And/or hydroxyl zinc complex.
The second aspect of the present invention is to provide the preparation method of the heat stabilizer, the method comprise the following steps at least
It is a kind of：
(1) hydroxy compounds, zinc compound are uniformly mixed, and 2-10h is heated at 130-200 DEG C, by gained
Mixture adds low-carbon alcohols after being cooled to 25-60 DEG C, form uniform slurry, by slurry centrifugation, washing, dries, and obtains
Hydroxyl zinc complex；
(2) calcium containing compound, hydroxy compounds and low-carbon alcohols are well mixed, 1- is reacted under the counterflow condition of low-carbon alcohols
10h, is cooled to suction filtration, washing, drying after room temperature, obtains hydroxyl calcium complex.
The third aspect of the present invention is to provide a kind of composite thermal stabilizer, and the composite thermal stabilizer includes main stabilizer and auxiliary
Heat stabilizer is helped, the main stabilizer is (0.8-2) with the weight ratio of auxiliary heat stabilizer：(0.9-2)；Wherein, the master is steady
Determine agent for above-mentioned hydroxo complex heat stabilizer, the auxiliary heat stabilizer be zinc soap, calcium soap, polyalcohol, hydrotalcite, zeolite and
At least one in beta-diketon.
The fourth aspect of the present invention provides a kind of poly (vinyl chloride) resin composition, and said composition includes following components：
The Corvic of 100 weight portions；
The composite thermal stabilizer of 1.5-4 weight portions；
The lubricant of 0.2-0.4 weight portions；
The plasticizer of 0-5 weight portions；
Wherein, the composite thermal stabilizer is above-mentioned composite thermal stabilizer.
The fifth aspect of the present invention is to provide the preparation method of above-mentioned poly (vinyl chloride) resin composition, and the method includes, will
Composite thermal stabilizer, lubricant and plasticizer mixed at high speed, and plasticizing is kneaded, then mix with Corvic again.
The advantage of the invention is that prepared composite thermal stabilizer is used for the stabilizer of the plastic processings such as PVC, with not
Easily separate out, the characteristics of nontoxic, cheap, stablizing effect is good.Composite thermal stabilizer prepared by the addition present invention can reduce PVC systems
The counter balance torque of product, improves processing characteristics, reduces cost.By the PVC to addition hydroxyl calcium/zinc complex composite thermal stabilizer
Static burn in experiment is carried out, is as a result shown, adding composite thermal stabilizer of the invention can be obviously improved the heat endurance of PVC.
And preparation method of the invention is pollution-free, energy consumption is low, whole method is green, environmentally friendly, easy to operate, will not etching apparatus.
Specific embodiment
The present invention provides a kind of hydroxo complex heat stabilizer, and the heat stabilizer is hydroxyl calcium complex and/or hydroxyl zinc
Complex compound；Preferably hydroxyl zinc complex, more preferably hydroxyl calcium complex and hydroxyl zinc complex, most preferably weight
Than being 1：The hydroxyl calcium complex and hydroxyl zinc complex of 1-5.With the use of the hydroxyl calcium complex and hydroxyl of aforementioned proportion scope
Base zinc complex can further improve the stability of heat stabilizer.
It was found by the inventors of the present invention that containing 1 to 8 hydroxyl, wherein hydroxyl and calcium or zinc shape in working as the heat stabilizer
During into corresponding calcium oxygen key or zinc oxygen key, the stability of the hydroxo complex heat stabilizer is preferable.This is due to calcium
The hydroxo complex of oxygen key or zinc oxygen key has unstable structure, the work of substitution unstable chlorine atom in passivation polyvinyl chloride chain
With so as to delay the degraded of polyvinyl chloride, improve the heat endurance of polyvinyl chloride.When heat stabilizer is hydroxyl calcium complex
During with hydroxyl zinc compound, in terms of the total hydroxy of the two.
The present invention provides the preparation method of above-mentioned heat stabilizer, the method comprise the following steps at least one：
(1) hydroxy compounds, zinc compound are uniformly mixed, and 2-10h is heated at 130-200 DEG C, by gained
Mixture adds low-carbon alcohols after being cooled to 25-60 DEG C, form uniform slurry, by slurry centrifugation, washing, dries, and obtains
Hydroxyl zinc complex；
(2) calcium containing compound, hydroxy compounds and low-carbon alcohols are well mixed, 1- is reacted under the counterflow condition of low-carbon alcohols
10h, is cooled to suction filtration, washing, drying after room temperature, obtains hydroxyl calcium complex.
In the case of with the use of hydroxyl zinc complex and hydroxyl calcium complex, hydroxyl is obtained respectively according to above-mentioned steps
The two is mixed after zinc complex and hydroxyl calcium complex.
According to the present invention, the hydroxy compounds is preferably in pentaerythrite, bipentaerythrite, mannitol and sorbierite
It is at least one.
In the present invention, low-carbon alcohols function as hydroxyl source and solvent, therefore, this area conventional various low-carbon alcohols
It is capable of achieving the purpose.Preferably, the low-carbon alcohols are the alcohol of carbon number 1-5, more preferably methyl alcohol, ethanol and isopropyl
At least one in alcohol；Most preferably isopropanol.
In the present invention, the zinc compound and calcium containing compound are the sources as zinc and calcium.The zinc compound
With the oxide or various inorganic salts that calcium containing compound can be zinc and calcium.Preferably, the zinc compound is zinc oxide, carbon
At least one in sour zinc, zinc chloride, zinc acetate, zinc nitrate and zinc sulfate；The calcium containing compound be calcium oxide, calcium carbonate,
At least one in calcium chloride, calcium nitrate, calcium sulfite and calcium sulfate.
According to the present invention, to obtain above-mentioned preferred hydroxyl calcium complex and hydroxyl zinc complex, hydroxyl described in step (1)
The weight ratio preferably 1 of based compound, zinc compound and low-carbon alcohols：0.1-0.5：0.5-1.0, more preferably 1：0.2-
0.4：0.6-0.8；The weight ratio preferably 1 of hydroxy compounds, calcium containing compound and low-carbon alcohols described in step (2)：0.05-
0.25：0.25-0.5, more preferably 1：0.08-0.2：0.3-0.4.
Low-carbon alcohols are added preferably to mix a period of time according to the present invention, in step (1), such as 10-30min is uniform to be formed
Slurry.
According to the present invention, in step (1), the centrifugation, washing, drying are the conventional purification process in this area.It is above-mentioned
Washing preferably uses low-carbon (LC) alcohol organic solvent, for example, at least one in methyl alcohol, ethanol and isopropanol.
Similarly, suction filtration described in step (2), washing, drying also can be the conventional method in this area.The washing is excellent
Choosing uses low-carbon (LC) alcohol organic solvent, for example, at least one in methyl alcohol, ethanol and isopropanol.
The present invention provides a kind of composite thermal stabilizer, and the composite thermal stabilizer includes main stabilizer and auxiliary heat stabilizer,
The main stabilizer is (0.8-2) with the weight ratio of auxiliary heat stabilizer：(0.9-2)；Wherein, the main stabilizer is above-mentioned hydroxyl
Base complex heat stabilizer, the auxiliary heat stabilizer be zinc soap, calcium soap, polyalcohol, hydrotalcite, zeolite and beta-diketon in extremely
Few one kind.
Preferably, the zinc soap is at least one in zinc stearate, zinc laurate and zinc palmitate.
Preferably, the calcium soap is at least one in calcium stearate, calcium laurate and calcium palmitate.
Preferably, the polyalcohol is at least one in pentaerythrite, bipentaerythrite, mannitol and sorbierite.
The present invention provides a kind of poly (vinyl chloride) resin composition, and said composition includes following components：
The Corvic of 100 weight portions；
The composite thermal stabilizer of 1.5-4 weight portions；
The lubricant of 0.2-0.4 weight portions；
The plasticizer of 0-5 weight portions；
Wherein, the composite thermal stabilizer is above-mentioned composite thermal stabilizer.
According to the present invention, the lubricant and plasticizer can be the conventional selection of this area.
The fifth aspect of the present invention is to provide the preparation method of above-mentioned poly (vinyl chloride) resin composition, and the method includes, will
Composite thermal stabilizer, lubricant and plasticizer mixed at high speed, and plasticizing is kneaded, then mix with Corvic again.Wherein,
Mixed at high speed, the actual conditions of mixing plasticizing can be this area normal condition.
The present invention will be further described with reference to embodiments.
Embodiment 1
According to mass ratio 120：30：1 weighs hydroxy compounds, zinc oxide, zinc carbonate, is sufficiently mixed three until obtaining
Uniform slurry.Slurry is heated at a temperature of 130 DEG C, and uniform Hybrid Heating 3h at such a temperature.Mixture is cooled to
40 DEG C and isopropanol mixing 15min is added, form uniform slurry.Slurry is centrifuged 30min, washed with isopropanol, be centrifuged,
Dry, obtain final product hydroxyl zinc complex.
By 40 mass parts hydroxyl zinc complexes, 20 mass parts calcium stearates, 20 mass parts zeolites, 4 mass parts beta-diketons, 8
Mass parts bipentaerythrite and 8 mass parts PE wax mixed at high speed 5min, then knead 4-5min, bar of plasticating in two-roll mill
Part is preliminary roller rotating speed 18r/min, back roller rotating speed 20r/min, 170 DEG C of roller temperature, bottom sheet after plasticizing completely.
Embodiment 2
60g calcium oxide is added in the methanol solution of 180g hydroxy compounds, stirring is allowed to well mixed.Then in first
3.5h is reacted under the counterflow condition of alcohol.Room temperature is cooled to, suction filtration washs 3 times with ethanol, then in being dried under vacuum to perseverance at 60 DEG C
Weight, obtains hydroxyl calcium complex.
By 40 mass parts zinc stearates, 20 mass parts hydroxyl calcium complexs, 20 mass parts zeolites, 4 mass parts beta-diketons, 8
Mass parts bipentaerythrite and 8 mass parts PE wax mixed at high speed 5min, then knead 4-5min, bar of plasticating in two-roll mill
Part is preliminary roller rotating speed 18r/min, back roller rotating speed 20r/min, 170 DEG C of roller temperature, bottom sheet after plasticizing completely.
Embodiment 3
According to mass ratio 120：30：1 weighs hydroxy compounds, zinc oxide, zinc carbonate, is sufficiently mixed three until obtaining
Uniform slurry.Slurry is heated at a temperature of 150 DEG C, and uniform Hybrid Heating 4h at such a temperature.Mixture is cooled to
40 DEG C and isopropanol mixing 15min is added, form uniform slurry.Slurry is centrifuged 30min, washed with isopropanol, be centrifuged,
Dry, obtain final product hydroxyl zinc complex.
60g calcium oxide is added in the methanol solution of 200g hydroxy compounds, stirring is allowed to well mixed.Then in first
2.5h is reacted under the counterflow condition of alcohol.Room temperature is cooled to, suction filtration washs 3 times with ethanol, then in being dried under vacuum to perseverance at 60 DEG C
Weight, obtains hydroxyl calcium complex.
By 40 mass parts hydroxyl zinc complexes, 20 mass parts hydroxyl calcium complexs, 20 mass parts zeolites, 4 mass parts β-two
Ketone, 8 mass parts bipentaerythrites and 8 mass parts PE wax mixed at high speed 5min, then knead 4-5min in two-roll mill, modeling
Refining condition is preliminary roller rotating speed 18r/min, back roller rotating speed 20r/min, 170 DEG C of roller temperature, bottom sheet after plasticizing completely.
Comparative example 1
By the glycerin zinc shown in 40 mass parts Formulas I, 20 mass parts calcium stearates, 20 mass parts zeolites, 4 mass parts β-two
Ketone, 8 mass parts bipentaerythrites and 8 mass parts PE wax mixed at high speed 5min, then knead 4-5min in two-roll mill, modeling
Refining condition is preliminary roller rotating speed 18r/min, back roller rotating speed 20r/min, 170 DEG C of roller temperature, bottom sheet after plasticizing completely.
Comparative example 2
By the glycerine calcium shown in 40 mass parts zinc stearates, 20 mass parts Formula II, 20 mass parts zeolites, 4 mass parts β-two
Ketone, 8 mass parts bipentaerythrites and 8 mass parts PE wax mixed at high speed 5min, then knead 4-5min in two-roll mill, modeling
Refining condition is preliminary roller rotating speed 18r/min, back roller rotating speed 20r/min, 170 DEG C of roller temperature, bottom sheet after plasticizing completely.
The stability of composite thermal stabilizer of the invention is tested below by way of test case.Will be compound thermally-stabilised
Agent, dioctyl phthalate (DOP), polyvinyl chloride (PVC) resin are plasticated in flakes, according to national standard on twin-roll plastic mixing mill
GB/T2917.1-2002 congo red methods, determine the static heat stability energy of the mixture of PVC and heat stabilizer.
Test case 1：Congo Red test
The mass parts of composite thermal stabilizer 2.5 prepared by above-described embodiment 1,2 and 3 are added separately to 100 mass parts PVC
In, Congo Red test is carried out after being sufficiently mixed, as a result as shown in table 1.Wherein, commercially available low lead heat stabilizer is the intelligent section's auxiliary agent in Shandong
The low lead heat stabilizers of HKW-104 of production.
Table 1
| Test case | Heat stabilizer (part) | PVC (part) | Coloring Time (minute) |
| 1-1 | Composite thermal stabilizer (2.5) obtained in embodiment 1 | 100 | 46 |
| 1-2 | Composite thermal stabilizer (2.5) obtained in embodiment 2 | 100 | 20 |
| 1-3 | Composite thermal stabilizer (2.5) obtained in embodiment 3 | 100 | 48 |
| Contrast test example | |||
| 1-4 | Commercially available low lead heat stabilizer (2.5) | 100 | 16 |
| 1-5 | Composite thermal stabilizer (2.5) obtained in comparative example 1 | 100 | 14 |
| 1-6 | Composite thermal stabilizer (2.5) obtained in comparative example 2 | 100 | 15 |
Test case 2：Baking oven thermal aging test
The mass parts of composite thermal stabilizer 2.5 prepared by above-described embodiment 1,2 and 3 are respectively added to 100 mass parts PVC
In, 50 mass parts diisooctyl phthalates (DOP) are added, kneaded 10 minutes in 140 DEG C in plastics experimental machine,
160 DEG C of conditions depress to thickness for the thin slice of 1mm and are cut into the test piece of 1cm × 1cm.The heat that test piece is placed in into 180 DEG C ± 1 DEG C is old
Change chamber in carry out static burn in experiment, by test piece start and occur black decomposition point time be set to heat-stable time (point
Clock).The results are shown in Table 2.Wherein test case 2-4 is the comparative example of not heat stabilizers.
Table 2
Can be found from Tables 1 and 2, the use composite thermal stabilizer according to prepared by the present invention is thermally-stabilised with traditional lead salt
Agent and prior art other heat stabilizers compare with outstanding heat endurance.
Contrast Tables 1 and 2 can be seen that composite thermal stabilizer simultaneously using hydroxyl zinc complex and hydroxyl calcium complex
With more preferable heat endurance.
It is described above various embodiments of the present invention, described above is exemplary, and non-exclusive, and
It is not limited to disclosed each embodiment.In the case of without departing from the scope and spirit of illustrated each embodiment, for this skill
Many modifications and changes will be apparent from for the those of ordinary skill in art field.
Claims (8)
1. a kind of hydroxo complex heat stabilizer, it is characterised in that the heat stabilizer is that weight ratio is 1：The hydroxyl calcium complexing of 1-5
Thing and hydroxyl zinc complex；
Wherein, the preparation method of the hydroxyl zinc complex is comprised the following steps：Hydroxy compounds, zinc compound are uniformly mixed
Close, and 2-10h is heated at 130-200 DEG C, low-carbon alcohols are added after the mixture of gained is cooled into 25-60 DEG C, form uniform
Slurry, by the slurry centrifugation, washing, dry, obtain hydroxyl zinc complex；
The preparation method of the hydroxyl calcium complex is comprised the following steps：Calcium containing compound, hydroxy compounds and low-carbon alcohols are mixed
Close uniform, 1-10h is reacted under the counterflow condition of low-carbon alcohols, be cooled to suction filtration, washing, drying after room temperature, obtain hydroxyl calcium network
Compound；
The hydroxy compounds is at least one in pentaerythrite, bipentaerythrite, mannitol and sorbierite；
The low-carbon alcohols are the alcohol of carbon number 1-5；
The zinc compound is at least one in zinc oxide, zinc carbonate, zinc chloride, zinc acetate, zinc nitrate and zinc sulfate；
The calcium containing compound is at least one in calcium oxide, calcium carbonate, calcium chloride, calcium nitrate, calcium sulfite and calcium sulfate；
Contain 1 to 8 hydroxyl in the heat stabilizer, wherein hydroxyl forms corresponding calcium oxygen key or zinc oxygen key with calcium or zinc.
2. heat stabilizer according to claim 1, wherein, the low-carbon alcohols be in methyl alcohol, ethanol and isopropanol at least
It is a kind of.
3. heat stabilizer according to claim 1, wherein, in the preparation method of the hydroxyl zinc complex, the hydroxyl
The weight ratio of compound, zinc compound and low-carbon alcohols is 1：0.1-0.5：0.5-1.0；The preparation side of the hydroxyl calcium complex
In method, the weight ratio of the hydroxy compounds, calcium containing compound and low-carbon alcohols is 1：0.05-0.25：0.25-0.5.
4. the preparation method of the heat stabilizer as described in any one in claim 1-3, it is characterised in that the method include with
Lower step：
(1) hydroxy compounds, zinc compound are uniformly mixed, and 2-10h is heated at 130-200 DEG C, by the mixing of gained
Thing adds low-carbon alcohols after being cooled to 25-60 DEG C, form uniform slurry, by slurry centrifugation, washing, dries, and obtains hydroxyl
Zinc complex；
(2) calcium containing compound, hydroxy compounds and low-carbon alcohols are well mixed, 1-10h are reacted under the counterflow condition of low-carbon alcohols,
Suction filtration, washing, drying after room temperature are cooled to, hydroxyl calcium complex is obtained.
5. a kind of composite thermal stabilizer, it is characterised in that the composite thermal stabilizer includes main stabilizer and auxiliary heat stabilizer, institute
It is (0.8-2) that main stabilizer is stated with the weight ratio of auxiliary heat stabilizer：(0.9-2)；Wherein, the main stabilizer is claim
Hydroxo complex heat stabilizer in 1-3 described in any one, the auxiliary heat stabilizer is zinc soap, calcium soap, polyalcohol, neatly
At least one in stone, zeolite and beta-diketon.
6. composite thermal stabilizer according to claim 5, wherein, the zinc soap is zinc stearate, zinc laurate and palm
At least one in sour zinc；The calcium soap is at least one in calcium stearate, calcium laurate and calcium palmitate；The polyalcohol
It is at least one in pentaerythrite, bipentaerythrite, mannitol and sorbierite.
7. a kind of poly (vinyl chloride) resin composition, it is characterised in that said composition includes following components：
The Corvic of 100 weight portions；
The composite thermal stabilizer of 1.5-4 weight portions；
The lubricant of 0.2-0.4 weight portions；
The plasticizer of 0-5 weight portions；
Wherein, the composite thermal stabilizer is the composite thermal stabilizer described in claim 5 or 6.
8. the preparation method of poly (vinyl chloride) resin composition as claimed in claim 7, it is characterised in that the method includes, will
Composite thermal stabilizer, lubricant and plasticizer mixed at high speed, and plasticizing is kneaded, then mix with Corvic again.
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