CN108752638B - High-efficiency powder heat stabilizer, preparation method thereof and application thereof in ultra-transparent PVC (polyvinyl chloride) products - Google Patents
High-efficiency powder heat stabilizer, preparation method thereof and application thereof in ultra-transparent PVC (polyvinyl chloride) products Download PDFInfo
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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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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- 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
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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
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
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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
- C08K5/09—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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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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
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
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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
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
Abstract
The invention discloses a high-efficiency powder heat stabilizer, a preparation method thereof and application thereof in an ultra-transparent PVC product. The high-efficiency powder heat stabilizer is prepared from 50-80 parts of superfine hydrotalcite, 1-5 parts of coupling agent, 8-20 parts of zinc salt, 3-8 parts of mosaic, 5-15 parts of beta-diketone, 1-5 parts of antioxidant and 0-10 parts of silicon dioxide. The compatibility of the heat stabilizer and PVC powder is obviously improved, and the PVC product has more excellent heat stability, weather resistance and transparency. Is suitable for PVC transparent and ultra-transparent products.
Description
Technical Field
The invention relates to a heat stabilizer, in particular to a high-efficiency powder heat stabilizer and application thereof in an ultratransparent PVC product.
Background
At present, most domestic transparent products mainly use organic tin heat stabilizers, but the organic tin is expensive, most varieties have bad smell, and tin belongs to heavy metals, so that the problem of toxicity is controversial. Other transparent heat stabilizers are mainly liquid stabilizers, and the solvents are complex and various, so that the plasticizing problem of the product is influenced negatively. The research and application of the zinc-based transparent heat stabilizer powder in China are few.
The domestic powdered zinc-based heat stabilizer is prepared by blending and compounding a plurality of raw materials and can meet the application requirements of general products. Under the condition of transparent and long-acting stability requirements, a large amount of hydrotalcite is filled to improve the performance. Although the hydrotalcite has certain improvement on the performance, the hydrotalcite is an inorganic substance and has poor compatibility with PVC powder, so that uneven dispersion is easy to generate when the filling amount is large, a product is brittle, the mechanical property is reduced, and the transparency and the stability of the product cannot meet the requirements.
Disclosure of Invention
The invention aims to provide a high-efficiency powder heat stabilizer capable of improving the heat stability and transparency of PVC products.
The technical scheme adopted by the invention is as follows: a high-efficiency powder heat stabilizer is prepared from the following raw materials in parts by weight:
preferably, the superfine hydrotalcite is aluminum-magnesium binary hydrotalcite, wherein the molar ratio of MgO to Al is2O31 in terms of (3-5), and the particle size of the hydrotalcite is 0.3-0.5 micron.
Preferably, the coupling agent has the following structure,
wherein, B is ligand molecule, which is one of ethylenediamine or ethylamine; a. b is polymerization degree, a + b is less than or equal to 5; r is one of lauryl alcohol, stearyl alcohol, lauric acid or stearic acid.
Preferably, the zinc salt is zinc stearate or zinc isooctanoate.
Preferably, the beta-diketone is one or two of dibenzoyl methane, stearoyl benzoyl methane and calcium acetylacetonate.
Preferably, the antioxidant is one or two of [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, tris [2, 4-di-tert-butylphenyl ] phosphite, dilauryl thiodipropionate and triphenyl phosphite.
Preferably, the silica is fumed silica.
Preferably, the method comprises the following steps: premixing the coupling agent and the superfine hydrotalcite by a high-speed mixer, controlling the temperature to be 100-110 ℃, and then sequentially adding the zinc salt, the mosaic, the beta-diketone, the antioxidant and the silicon dioxide according to the formula for mixing.
The high-efficiency powder heat stabilizer is applied to an ultra-transparent PVC product. According to the weight portion, 90-110 portions of PVC, 1-4 portions of the high-efficiency powdery heat stabilizer and 30-50 portions of dioctyl phthalate (DOP) are mixed in a double-roller mixing mill, the temperature of the double rollers is set to be 180 ℃, the rotating speed is 21r/min, the mixing time of the double rollers is 5min, the mixture is tabletted after mixing, the temperature of a tabletting machine is set to be 170 ℃, and the tabletting time is 3min, so that the ultra-transparent PVC product is obtained.
The invention has the beneficial effects that: the invention obtains the high-efficiency heat stabilizer by compounding the coupling agent modified hydrotalcite and other auxiliary materials, and the heat stabilizer provided by the invention has the following characteristics: (1) excellent compatibility with PVC products (2) excellent stability and transparency. (3) The powder heat stabilizer is non-toxic and environment-friendly, and has low cost.
Detailed Description
The present invention is further illustrated in detail by the following examples, which are provided to facilitate the understanding of those skilled in the art, and are not intended to limit the scope of the present invention. In the following examples of the present invention,
example 1
The formula (I) is as follows: is prepared from the following raw materials in part by weight
Superfine hydrotalcite: 60kg of
Coupling agent: 3kg of
Zinc isooctoate: 17kg of
And (3) mosaic: 7kg of
Dibenzoylmethane: 6kg of
Pentaerythritol beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate: 1kg of
Tris [2, 4-di-tert-butylphenyl ] phosphite: 1kg of
Silicon dioxide: 5kg of
The superfine hydrotalcite is aluminum-magnesium binary hydrotalcite, wherein the molar ratio of MgO to Al is2O3Hydrotalcite particle size was 0.43 microns ═ 4.3: 1.
The structure of the coupling agent is as follows,
wherein, B is ligand molecule ethylamine; a. b is the degree of polymerization, a + b is 5; r is lauryl alcohol.
(II) preparation method
Firstly, adding superfine hydrotalcite and a coupling agent into a high-speed mixer, starting the equipment, controlling the rotating speed to be 750r/min, opening a cooling device of the high-speed mixer when the temperature is 100 ℃, slowly dripping zinc isooctanoate, and continuing to rotate for 5min after dripping. Opening the high-speed mixer, adding other raw materials, closing the cooling device, starting to rotate at high speed, controlling the rotation speed at 1500r/min and the temperature at 105 ℃, stirring for 10min, stopping the machine, and inspecting and packaging when the temperature is reduced to below 50 ℃.
Example 2
The formula (I) is as follows: is prepared from the following raw materials in part by weight
Superfine hydrotalcite: 60kg of
Coupling agent: 3kg of
Zinc stearate: 17kg of
And (3) mosaic: 7kg of
Dibenzoylmethane: 6kg of
Pentaerythritol beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate: 1kg of
Tris [2, 4-di-tert-butylphenyl ] phosphite: 1kg of
Silicon dioxide: 5kg of
The superfine hydrotalcite is aluminum-magnesium binary hydrotalcite, wherein the molar ratio of MgO to Al is2O3Hydrotalcite particle size was 0.38 microns ═ 4.21: 1.
The structure of the coupling agent is as follows,
wherein, B is ligand molecule ethylenediamine; a. b is the degree of polymerization, a + b is 5; r is stearyl alcohol.
(II) preparation method
Firstly, adding superfine hydrotalcite and a coupling agent into a high-speed mixer, starting the equipment, controlling the rotating speed to be 750r/min, stopping the machine when the temperature rises to 100 ℃, starting the high-speed mixer, and adding other raw materials. Continuously starting high-speed rotation, controlling rotation speed at 1500r/min and temperature at 105 deg.C, stirring for 15min, stopping machine, cooling to below 50 deg.C, inspecting, and packaging.
Example 3
The formula (I) is as follows: is prepared from the following raw materials in part by weight
Superfine hydrotalcite: 65kg of
Coupling agent: 3kg of
Zinc stearate: 17kg of
And (3) mosaic: 7kg of
Dibenzoylmethane: 6kg of
Pentaerythritol beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate: 1kg of
Tris [2, 4-di-tert-butylphenyl ] phosphite: 1kg of
Silicon dioxide: 0kg of
The superfine hydrotalcite is aluminum-magnesium binary hydrotalcite, wherein the molar ratio of MgO to Al is2O3Hydrotalcite particle size was 0.38 microns ═ 4.21: 1.
The structure of the coupling agent is as follows,
wherein, B is ligand molecule ethylenediamine; a. b is the degree of polymerization, a + b is 5; r is stearic acid.
(II) preparation method
Firstly, adding superfine hydrotalcite and a coupling agent into a high-speed mixer, starting the equipment, controlling the rotating speed to be 750r/min, stopping the machine when the temperature rises to 100 ℃, starting the high-speed mixer, and adding other raw materials. And (4) continuously starting high-speed rotation, controlling the rotation speed to be 1500r/min, controlling the temperature to be 105 ℃, stirring for 15min, stopping the machine, and checking and packaging when the temperature is reduced to be below 50 ℃.
Example 4 application
The heat stabilizers prepared in examples 1-3 were compared with those prepared in comparative examples in terms of their properties, including heat stability, transparency, colorability and aging properties.
Comparative example
1. The formula is as follows: is prepared from the following raw materials in part by weight
Superfine hydrotalcite: 60kg of
Zinc stearate: 17kg of
And (3) mosaic: 7kg of
Dibenzoylmethane: 6kg of
Pentaerythritol beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate: 1kg of
Tris [2, 4-di-tert-butylphenyl ] phosphite: 1kg of
Silicon dioxide: 8kg of
The superfine hydrotalcite is aluminum-magnesium binary hydrotalcite, wherein the molar ratio of MgO to Al is2O3Hydrotalcite particle size was 0.43 microns ═ 4.3: 1.
2. The preparation method comprises the following steps: firstly, adding superfine hydrotalcite and a coupling agent into a high-speed mixer, starting the equipment, controlling the rotating speed to be 750r/min, stopping the machine when the temperature rises to 100 ℃, starting the high-speed mixer, and adding other raw materials. And (4) continuously starting high-speed rotation, controlling the rotation speed to be 1500r/min, controlling the temperature to be 105 ℃, stirring for 15min, stopping the machine, and checking and packaging when the temperature is reduced to be below 50 ℃.
(II) PVC products were prepared using the heat stabilizers prepared in examples 1-3 and comparative example.
1. The following formula is selected as the experimental formula for PVC products:
100g of PVC, 3g of stabilizer and 40g of DOP.
2. The process for making the PVC article is as follows: the double-roller tabletting process is adopted, the temperature of the double rollers is set to be 180 ℃, the rotating speed is 21r/min, and the double-roller mixing time is 5 min. Mixing, tabletting, and shaping with 1mm mold, wherein the temperature of the tabletting machine is set to 170 deg.C, and the tabletting time is 3 min.
3. Detection of
1) The two-roll dynamic thermal ageing was carried out continuously using the two-roll conditions, the dynamic thermal stability of the stabilizer was analyzed by observing the time the coupon changes color, and the time it took for the coupon to eventually ash was recorded. The results are shown in Table 1.
2) The transparency test method of the PVC sample sheets prepared in examples 1-3 and comparative example is as follows: the transparency of the 1mm sheet pressed by the above two-roll kneader was measured in accordance with GB/T2910-2008, and the results of the transparency measurement are shown in Table 1.
3) The heat resistance test conditions of the PVC sample sheets prepared in examples 1 to 3 and comparative example were as follows: the heat resistance of the PVC sheet pressed by the double-roll rubber mixing mill is tested according to the GB/T9349-2002 standard, the test temperature is 190 ℃, and the initial coloring result grades are divided into several grades. Colorless, slightly yellow, light yellow, red, brown, gray, black, respectively, and the time to final sample darkening was recorded. The experimental data are shown in table 2.
TABLE 1 twin roll dynamic Heat aging time and transparency test results
| Test items | Example 1 | Example 2 | Example 3 | Comparative example |
| Double roller dynamic ageing time/min | 29 | 32 | 29 | 22 |
| Transmittance (a) | 98 | 96 | 95 | 90 |
As can be seen from Table 1, the dynamic thermal aging performance and light transmittance of the heat stabilizer product synthesized by the method are obviously superior to those of the stabilizer sample prepared by unmodified hydrotalcite. The stabilizer sample prepared from the modified hydrotalcite can obviously improve the performances of dynamic thermal aging, light transmittance and the like of the product, wherein the dynamic thermal stability time of the embodiment 2 is up to 32min, and the light transmittance of the embodiment 1 is up to 98%.
Table 2 thermal aging resistance test results using a thermal oven are as follows
| Time/min | Example 1 | Example 2 | Example 3 | Comparative example |
| 20 | Colorless and colorless | Colorless and colorless | Colorless and colorless | Colorless and colorless |
| 40 | Colorless and colorless | Colorless and colorless | Colorless and colorless | Light yellow |
| 50 | Colorless and colorless | Colorless and colorless | Light yellow | Light yellow |
| 60 | Colorless and colorless | Light yellow | Light yellow | Yellow colour |
| 70 | Light yellow | Light yellow | Yellow colour | Red colour |
| 80 | Yellow colour | Yellow colour | Red colour | Brown colour |
| 90 | Brown colour | Brown colour | Black color | Black color |
| 100 | Black color | Black color | Black color | Black color |
As can be seen from table 2, the initial coloration and the time to failure of examples 1, 2 and 3 are significantly better than those of the stabilizer samples prepared using unmodified hydrotalcite.
The heat stabilizer product prepared from the modified hydrotalcite is obviously improved in static heat stability, dynamic heat stability, transparency, colorability and the like. The modified hydrotalcite transparent heat stabilizer product prepared by the invention shows good stability and transparency in PVC product application.
Claims (7)
1. The efficient powder heat stabilizer is characterized by being prepared from the following raw materials in parts by weight:
50-80 parts of superfine hydrotalcite,
1-5 parts of coupling agent,
8-20 parts of zinc salt,
3-8 parts of mosaic,
5-15 parts of beta-diketone,
1-5 parts of antioxidant,
5-10 parts of silicon dioxide;
the superfine hydrotalcite is aluminum-magnesium binary hydrotalcite, wherein the molar ratio of MgO to Al is2O3= (3-5) = (1), particle size of hydrotalcite is 0.3-0.5 micron;
the structure of the coupling agent is as follows,
wherein, B is ligand molecule, which is one of ethylenediamine or ethylamine; a. b is polymerization degree, a + b is less than or equal to 5; r is one of lauryl alcohol, stearyl alcohol, lauric acid or stearic acid;
the silicon dioxide is fumed silicon dioxide.
2. The high efficiency powder heat stabilizer of claim 1, wherein the zinc salt is zinc stearate or zinc isooctanoate.
3. The efficient powder heat stabilizer of claim 1, wherein the beta-diketone is one or a combination of dibenzoylmethane, stearoylbenzoylmethane and calcium acetylacetonate.
4. The efficient powder heat stabilizer according to claim 1, wherein the antioxidant is one or a combination of two of [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] pentaerythritol ester, tris [2, 4-di-tert-butylphenyl ] phosphite, dilauryl thiodipropionate and triphenyl phosphite.
5. The preparation method of the high-efficiency powder heat stabilizer of claim 1, which is characterized by comprising the following steps: premixing the coupling agent and the superfine hydrotalcite by a high-speed mixer, controlling the temperature to be 100-110 ℃, and then sequentially adding the zinc salt, the mosaic, the beta-diketone, the antioxidant and the silicon dioxide according to the formula for mixing.
6. The use of the high efficiency powder heat stabilizer of claim 1 in ultra-transparent PVC products.
7. The use of claim 6, wherein the ultra-transparent PVC product is prepared by mixing 90-110 parts by weight of PVC, 1-4 parts by weight of the high efficiency powdery thermal stabilizer of claim 1 and 30-50 parts by weight of dioctyl phthalate in a two-roll mixer, wherein the two-roll temperature is 180 ℃, the rotation speed is 21r/min, the two-roll mixing time is 5min, the mixing is followed by tabletting, the tablet press temperature is 170 ℃, and the tabletting time is 3 min.
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| CN109721886A (en) * | 2018-12-28 | 2019-05-07 | 山东三义实业股份有限公司 | PVC environment friendly transparent zinc-base heat stabilizer and its preparation process |
| CN110330741A (en) * | 2019-07-25 | 2019-10-15 | 东莞市柯益信息技术有限公司 | A kind of environmental protection high transparency leaded light PVC is stabilizing agent specially used and preparation method thereof |
| CN111171584A (en) * | 2019-12-30 | 2020-05-19 | 安徽华文塑胶科技有限公司 | Stabilizer for PCB and preparation method thereof |
| CN113816842B (en) * | 2021-10-11 | 2022-04-12 | 山东键兴新材料科技有限公司 | Calcium acetylacetonate, preparation method and application thereof |
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| WO1996005140A1 (en) * | 1994-08-15 | 1996-02-22 | Aluminum Company Of America | Two powder synthesis of hydrotalcite and hydrotalcite-like compounds |
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