CN113444328B - PVC (polyvinyl chloride) main stabilizer, composite heat stabilizer for PVC and PVC - Google Patents
PVC (polyvinyl chloride) main stabilizer, composite heat stabilizer for PVC and PVC Download PDFInfo
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Abstract
The invention discloses a PVC (polyvinyl chloride) main stabilizer which is a rare earth complex with a benzophenone structure; compounding the heat stabilizer with an auxiliary stabilizer, namely stearate and/or polyalcohol to prepare a composite heat stabilizer for PVC; the composite heat stabilizer prepared by the invention has good heat stability and long-term discoloration resistance; the PVC pipe has excellent mechanical and processing properties in the aspect of actual production, has the characteristics of no toxicity and environmental protection, can be applied to the processing and manufacturing of PVC pipes, and has remarkable social and economic benefits.
Description
Technical Field
The invention relates to the field of high polymer materials, in particular to a PVC (polyvinyl chloride) main stabilizer, a PVC composite heat stabilizer and PVC.
Background
Polyvinyl chloride is one of five general-purpose plastics, and is widely applied to industries such as building, transportation, manufacturing, military and the like due to the characteristics of high strength, corrosion resistance, high insulation and the like. However, PVC has poor thermal stability, and when the processing temperature is above 100 ℃, due to the structural defects in the molecule, the PVC can generate zipper dehydrochlorination, so that the performances such as color change, mechanics and the like are poor, and the normal processing of the PVC is seriously influenced. Therefore, a heat stabilizer must be added during the processing, and the heat stabilizer can inhibit the generation of conjugated double bonds by substituting certain unstable chlorine atoms, such as allyl chloride and tertiary chlorine, in the long-chain structure of PVC. It can also absorb the hydrogen chloride generated by the degradation of PVC, thereby improving the thermal stability of PVC.
The heat stabilizers mainly used at present include lead salts, metal soaps, organic tin compounds and the like. However, lead salt type heat stabilizers contain heavy metals, cause environmental pollution, and remove PbSt 2 In addition, most lead salt thermal stabilizers are not conducive to use in transparent polyvinyl chloride. Although the organotin compound heat stabilizer can be used for transparent polyvinyl chloride and has excellent heat stability, it is expensive and contains a small amount of toxicity. The metal soap heat stabilizer has no influence on the environment, but is inferior in heat stability and processability. The invention discloses a novel rare earth complex with a benzophenone structure, which is used as a main stabilizer for producing PVC and compounded with an auxiliary stabilizer, namely stearate and/or polyalcohol to form a novel composite heat stabilizer for PVC so as to prepare high-performance PVC.
Disclosure of Invention
The invention aims to provide a brand new PVC main stabilizer, which is used as the main stabilizer for producing PVC and compounded with an auxiliary stabilizer, namely stearate and/or polyhydric alcohol to form a novel composite heat stabilizer for PVC, so as to prepare high-performance PVC.
The technical scheme adopted by the invention is as follows: a PVC main stabilizer is a rare earth complex with a benzophenone structure.
The rare earth element in the main stabilizer is any one or combination of more of lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd), samarium (Sm), europium (Eu), gadolinium (Gd), terbium (Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb), lutetium (Lu), yttrium (Y) and scandium (Sc).
The preparation method of the PVC main stabilizer comprises the following steps:
(1) dissolving a compound with a benzophenone structure in absolute ethyl alcohol to prepare a first solution; the preferred concentration of the first solution is 0.2-0.5 g/mL;
the compound with a benzophenone structure can be one or more of 2- (4-methylbenzoyl) benzoic acid, 4-hydroxybenzophenone, 2-benzoylbenzoic acid, 2-hydroxybenzophenone and 4-propenyloxy-2-hydroxybenzophenone;
(2) heating a rare earth salt solution to remove moisture, and then dissolving the rare earth salt solution in absolute ethyl alcohol to prepare a second solution; the preferred concentration of the second solution is 0.1-0.6 g/mL;
the rare earth salt solution can be any one of sulfuric acid rare earth salt, nitric acid rare earth salt and chloridized rare earth salt; the rare earth element is any one or combination of more of lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd), samarium (Sm), europium (Eu), gadolinium (Gd), terbium (Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb), lutetium (Lu), yttrium (Y) and scandium (Sc);
(3) slowly dropwise adding a sodium hydroxide ethanol solution into the first solution under the conditions of water bath and stirring to obtain a white flocculent intermediate product; preferably, the water bath temperature is 40-60 ℃, the stirring speed is 400-500r/min, and the reaction rate can be increased by stirring in the water bath environment; the preferable concentration of the sodium hydroxide ethanol solution is 1-2 mol/L;
then, continuously stirring for 15-30min, and slowly dripping the second solution until the white flocculent product disappears; the stirring is continued for 15-50min to ensure that the saponification reaction is more thorough; the second solution is a rare earth salt solution, and is slowly dripped to prevent the over-high local alkalinity from causing rare earth hydroxide precipitation to influence the yield of the reaction;
then, stirring is continuously carried out for 5-6h, so that the reaction is more thorough, and the yield of the complex is high; then filtering, evaporating and concentrating the filtrate, cooling and crystallizing;
(4) washing the obtained crystal with anhydrous ethanol and deionized water for 3-5 times respectively; the purpose of washing is to purify the complex, wherein, the washing with absolute ethyl alcohol is to remove unreacted rare earth salt, ligand and byproducts; the deionized water is used for washing to remove the generated sodium nitrate; finally, drying in a vacuum drying oven at 50-60 ℃ to obtain the PVC main stabilizer; too high a temperature may cause the product to decompose, and too low a temperature may result in too long a drying time for the product.
Preferably, the first solution, the second solution and the ethanol solution of sodium hydroxide should satisfy n (the first solution): n (second solution): n (sodium hydroxide ethanol solution) = 2-3.5: 1: 1-3, and the like. The proportion can prevent rare earth hydroxide from appearing and has higher reaction rate.
A composite heat stabilizer for PVC is prepared from PVC (polyvinyl chloride) as main stabilizer (1-10 wt. portions), polyol (1-5) and/or stearate (1-5) through high-speed mixing.
The polyhydric alcohol can be any one or combination of more of sorbitol, propylene glycol, glycerol, mannitol, ethylene glycol, pentaerythritol and dipentaerythritol.
The stearate can be any one or combination of zinc stearate, magnesium stearate, cerium stearate, aluminum stearate, iron stearate, calcium stearate and lanthanum stearate.
PVC is prepared by mixing PVC powder, composite heat stabilizer and DOP, and plasticizing and milling.
The invention has the beneficial effects that: the invention provides a brand new PVC main stabilizer, which is used as the main stabilizer for producing PVC and compounded with an auxiliary stabilizer, namely stearate and/or polyalcohol into a novel composite heat stabilizer for PVC to prepare high-performance PVC; the invention has the following characteristics
(1) The preparation method has the advantages of simple preparation process, short reaction time, stable chemical property, environmental protection, no pollution and industrial production conditions;
(2) when the prepared rare earth complex with the benzophenone structure is compounded with an auxiliary stabilizer for use, a good synergistic effect is generated, and the thermal stability and the discoloration resistance of PVC are well improved;
(3) the rare earth complex with the benzophenone structure can improve the processability of PVC resin, plays a certain plasticizing effect and hardly influences the transparency of PVC;
(4) due to excellent discoloration resistance and mechanical property after compounding, the composite material can be applied to the production and processing of PVC pipes, and has better social and economic benefits.
Drawings
FIG. 1 is a block flow diagram of the process of the present invention.
FIG. 2 is a comparison of the discoloration resistance of two experimental heat stabilizers.
Detailed Description
The invention is further illustrated by the following specific but non-limiting examples.
Example 1
Preparation of lanthanum 2-benzoylbenzoate:
(1) putting 13.56g of 2-benzoylbenzoic acid into a beaker filled with 200mL of absolute ethyl alcohol solution, and stirring under a constant-speed stirrer of 400r/min to completely dissolve the 2-benzoylbenzoic acid to prepare a solution 1 of 0.2 g/mL;
(2) weighing 14.8mL and 1.356mol/L lanthanum nitrate solution in a beaker according to the molar ratio of 2-benzoylformic acid =1:3, heating to remove water in the solution, and then adding absolute ethanol solution to prepare 0.2g/mL solution 2 for later use;
(3) slowly dripping 60mL of 1mol/L sodium hydroxide ethanol solution into the solution 1 under the conditions of water bath and stirring to obtain a white flocculent intermediate product; continuing stirring for 30min, and slowly dripping the solution 2 into the mixture to ensure that the white flocculent product disappears; continuously stirring for 6 hours, filtering, evaporating and concentrating the filtrate, cooling and crystallizing to obtain 2-benzoyl lanthanum benzoate;
(4) and (3) washing the obtained 2-benzoyl lanthanum benzoate with absolute ethyl alcohol and deionized water for 5 times respectively, and finally drying in a vacuum drying oven at the temperature of 60 ℃ to obtain the PVC main stabilizer.
Example 2
Preparation of lanthanum 2- (4-methylbenzoyl) benzoate
(1) Placing 20g of 2- (4-methylbenzoyl) benzoic acid into a beaker filled with 150mL of absolute ethyl alcohol solution, and stirring the 2- (4-methylbenzoyl) benzoic acid solution under a constant-speed stirrer of 500r/min to completely dissolve the 2- (4-methylbenzoyl) benzoic acid solution to prepare a solution 3 of 0.1 g/mL;
(2) according to the proportion of lanthanum chloride: 2- (4-methylbenzoyl) benzoic acid =1: weighing 28mL of 1mol/L lanthanum chloride solution in a beaker according to the molar ratio of 3, heating to remove water in the solution, and then adding an absolute ethyl alcohol solution to prepare a 0.2g/mL solution 4 for later use;
(3) slowly dripping 80mL of 1mol/L sodium hydroxide ethanol solution into the solution 3 under the conditions of water bath and stirring to obtain a white flocculent intermediate product, continuously stirring for 40min, slowly dripping the solution 4 into the solution, and allowing the white flocculent product to disappear; continuing stirring for 5 hours, filtering, evaporating and concentrating the filtrate, cooling and crystallizing to obtain 2- (4-methylbenzoyl) lanthanum benzoate;
(4) washing the obtained 2- (4-methylbenzoyl) lanthanum benzoate with absolute ethyl alcohol and deionized water for 4 times respectively, and finally drying in a vacuum drying oven at 50 ℃ to obtain the PVC main stabilizer.
The prepared 2-lanthanum benzoylbenzoate and 2- (4-methylbenzoyl) lanthanum benzoate are weighed with an auxiliary stabilizer according to a certain weight ratio, and then the materials are mixed at a high speed to prepare the composite heat stabilizer. Some of the following examples are combinations of rare earth complexes with auxiliary stabilizers.
Example 3
16g of lanthanum 2-benzoylbenzoate and 4g of zinc stearate are mixed at a high speed for 5min to prepare the first composite heat stabilizer.
Example 4
10g of lanthanum 2-benzoylbenzoate and 6.66g of calcium stearate are mixed at a high speed for 5min to prepare a second composite heat stabilizer.
Example 5
And (3) mixing 14g of lanthanum 2-benzoylbenzoate and 9.33g of pentaerythritol at a high speed for 5min to obtain the third composite heat stabilizer.
Example 6
18g of lanthanum 2-benzoylbenzoate, 9g of calcium stearate and 18g of pentaerythritol are mixed at a high speed for 5min to prepare the compound heat stabilizer IV.
Example 7
12g of lanthanum 2-benzoylbenzoate, 12g of zinc stearate and 36g of pentaerythritol are mixed at a high speed for 5min to prepare the compound heat stabilizer V.
Example 8
14g of lanthanum 2- (4-methylbenzoyl) benzoate, 7g of calcium stearate and 14g of pentaerythritol are mixed at a high speed for 5min to prepare the six composite heat stabilizers.
Example 9
13g of lanthanum 2- (4-methylbenzoyl) benzoate, 13g of zinc stearate and 39g of pentaerythritol are mixed at a high speed for 5min to prepare the compound heat stabilizer seven.
The seven prepared composite heat stabilizers are used for further preparing PVC, and the process flow is as follows: 100 parts of PVC, 4 parts of composite heat stabilizer and 35 parts of DOP are mixed on a high-speed mixer, and then poured on a double-roller open mill with the set temperature of 180 ℃ and the roller spacing of 3mm for plasticizing and open milling for 5min to prepare the PVC sheet.
Experiment one
The prepared examples were compared to several other conventional heat stabilizers for heat stabilization time, and the test methods were as follows: congo Red test (in GB/T2917.1-2002 standard): fully grinding a certain amount of PVC powder and a heat stabilizer (the heat stabilizer accounts for 4% of the mass of PVC), uniformly filling the ground PVC powder and the heat stabilizer into two small and medium test tubes, tying a wet Congo red test paper above the test tubes at a position 2cm away from a sample, putting the test tube into an oil bath at 180 ℃, and recording the time for the test paper to turn blue.
The test results are shown in table 1:
TABLE 1 comparison of thermal stability times for several thermal stabilizers
Experiment two
The prepared examples were compared to several other conventional heat stabilizers for discoloration resistance, as follows: thermal aging test: according to the test method of ASTM21152-67, a certain amount of PVC powder and a heat stabilizer (the heat stabilizer accounts for 4% of the mass of the PVC) are weighed, fully ground, uniformly filled into 8 porcelain boats, placed in a heat aging box at 180 ℃, and the color change is recorded every 5 minutes. The test results are shown in fig. 2.
Experiment one, two analysis
As can be seen from Table 1 and FIG. 2, the thermal stabilization time of the intermediate product, lanthanum 2-benzoylbenzoate and lanthanum 2- (4-methylbenzoyl) benzoate, of the composite thermal stabilizer is 16min and 18min, respectively. And has good long-term discoloration resistance compared with calcium stearate, zinc stearate and pentaerythritol. After being compounded with several auxiliary stabilizers, such as calcium stearate, zinc stearate and pentaerythritol, the compound also shows good synergistic effect. In examples 6 to 9, the stabilization time and discoloration resistance were significantly improved, while the thermal stabilization time was relatively short but the initial discoloration resistance was good in example 3, and the thermal stabilization time was different by 5min in examples 4 and 5, but example 5 had excellent long-term discoloration resistance and example 5 had good short-term discoloration resistance. Therefore, according to actual needs, if long-term anti-discoloration performance and relatively long thermal stability time are needed, the compound stabilizer of the embodiment 4 and the embodiment 6 can be selected, if good short-term discoloration resistance and relatively long thermal stability time are needed, the compound stabilizer of the embodiment 5 and the embodiment 6 can be selected, and if the best comprehensive thermal stability is needed, the compound stabilizer of the embodiment 7 and the embodiment 9 can be selected.
Experiment three
And (3) testing tensile property: 100 parts of PVC, 4 parts of heat stabilizer and 35 parts of DOP are mixed at a high speed, plasticized and milled for 5min on a double-roller milling machine with the set temperature of 180 ℃ and the roller spacing of 3mm, and the prepared PVC sheet is cut into dumbbell-shaped sample strips according to the test standard GB/T1040-2006 test for tensile property of plastics, wherein the thickness of the sample strips is 3mm, the width of the narrow part of the sample strips is 10mm, and the total length of the sample strips is 150 mm. The test was carried out on a CMT model 6503 universal tester with a tensile speed of 10mm/min, and the test was repeated at least five times for each sample.
The test results are shown in table 2 below:
analysis in experiment
As shown in the data in Table 2, the intermediate products of the composite heat stabilizer, namely lanthanum 2-benzoylbenzoate and lanthanum 2- (4-methylbenzoyl) benzoate, have better tensile strength and tensile strain at break than zinc stearate, calcium stearate and pentaerythritol. The 2-lanthanum benzoylbenzoate and the 2- (4-methylbenzoyl) lanthanum benzoate can enhance the mechanical property of PVC. Moreover, as shown in the table, the tensile strength of only example 3 is inferior to that of the intermediate product of the composite heat stabilizer, while the mechanical properties of other examples 4-9 are superior to those of lanthanum 2-benzoylbenzoate, lanthanum 2- (4-methylbenzoyl) benzoate, zinc stearate, calcium stearate, pentaerythritol, and the tensile strength and tensile strain at break, further showing that the rare earth complex has synergistic effect with the conventional heat stabilizer. And it can be seen that the composite stabilizers of examples 7 and 9 are best in tensile strength and tensile strain at break.
The combination of the three experiments shows that the product of the invention has excellent thermal stability (experiment one); better discoloration resistance (experiment two) and good mechanical properties (experiment three).
It is to be understood that the present invention has been described with reference to certain embodiments, and that various changes in the features and embodiments, or equivalent substitutions may be made therein by those skilled in the art without departing from the spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from the essential scope thereof. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.
Claims (7)
1. A PVC main stabilizer is characterized in that: the preparation method comprises the following steps:
(1) dissolving 2- (4-methylbenzoyl) benzoic acid or 2-benzoylbenzoic acid in absolute ethyl alcohol to prepare a first solution;
(2) heating a rare earth salt solution to remove moisture, and then dissolving the rare earth salt solution in absolute ethyl alcohol to prepare a second solution;
slowly dropwise adding a sodium hydroxide ethanol solution into the first solution under the conditions of water bath and stirring to obtain a white flocculent intermediate product; then, continuously stirring and slowly dripping the second solution until the white flocculent product disappears; continuously stirring; then filtering, evaporating and concentrating the filtrate, cooling and crystallizing; the rare earth element in the rare earth salt is any one or combination of more of lanthanum La, cerium Ce, praseodymium Pr, neodymium Nd, samarium Sm, europium Eu, gadolinium Gd, terbium Tb, dysprosium Dy, holmium Ho, erbium Er, thulium Tm, ytterbium Yb, lutetium Lu, yttrium Y and scandium Sc;
washing the obtained crystal with absolute ethyl alcohol and deionized water respectively; and finally, placing the PVC resin in a vacuum drying oven for drying to obtain the PVC main stabilizer.
2. A PVC primary stabilizer according to claim 1, characterized in that: the concentration of the first solution is 0.2-0.5 g/mL; the concentration of the second solution is 0.1-0.6 g/mL; the concentration of the sodium hydroxide ethanol solution is 1-2 mol/L.
3. A PVC primary stabilizer according to claim 1, characterized in that: the rare earth salt solution is any one of sulfuric acid rare earth salt, nitric acid rare earth salt and chloridized rare earth salt.
4. A composite heat stabilizer for PVC, which is characterized in that the composite heat stabilizer is prepared by mixing the main PVC stabilizer and the auxiliary stabilizer of any one of claims 1 to 3; 1-10 parts of PVC main stabilizer, and 1-5 parts of polyhydric alcohol or/and 1-5 parts of stearate as auxiliary stabilizer.
5. The composite heat stabilizer for PVC according to claim 4, wherein the polyol is any one or more of sorbitol, propylene glycol, glycerol, mannitol, ethylene glycol, pentaerythritol and dipentaerythritol.
6. The composite heat stabilizer for PVC according to claim 4, wherein the stearate is one or more selected from zinc stearate, magnesium stearate, cerium stearate, aluminum stearate, iron stearate, calcium stearate and lanthanum stearate.
7. A PVC composition, characterized in that the PVC composition is prepared by mixing the PVC composite heat stabilizer of claim 4 with PVC powder and DOP, and then plasticizing and roll-milling the mixture.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4102839A (en) * | 1975-01-10 | 1978-07-25 | Rhone-Poulenc Industries | Stabilization of vinyl chloride polymers |
| CN105295242A (en) * | 2015-11-18 | 2016-02-03 | 安徽华塑股份有限公司 | Hydrotalcite composite environmental protection stabilizer for PVC, and preparation method thereof |
| CN108948420A (en) * | 2018-07-10 | 2018-12-07 | 内蒙古科技大学 | Rare earth composite stabilizer and preparation method thereof for PVC |
| CN110330686A (en) * | 2019-05-09 | 2019-10-15 | 包头稀土研究院 | Rare earth composite stabilizer and its preparation method and application |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4102839A (en) * | 1975-01-10 | 1978-07-25 | Rhone-Poulenc Industries | Stabilization of vinyl chloride polymers |
| CN105295242A (en) * | 2015-11-18 | 2016-02-03 | 安徽华塑股份有限公司 | Hydrotalcite composite environmental protection stabilizer for PVC, and preparation method thereof |
| CN108948420A (en) * | 2018-07-10 | 2018-12-07 | 内蒙古科技大学 | Rare earth composite stabilizer and preparation method thereof for PVC |
| CN110330686A (en) * | 2019-05-09 | 2019-10-15 | 包头稀土研究院 | Rare earth composite stabilizer and its preparation method and application |
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