CN115895297A - Preparation method of modified wollastonite PVC stabilizer - Google Patents
Preparation method of modified wollastonite PVC stabilizer Download PDFInfo
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- CN115895297A CN115895297A CN202211640772.2A CN202211640772A CN115895297A CN 115895297 A CN115895297 A CN 115895297A CN 202211640772 A CN202211640772 A CN 202211640772A CN 115895297 A CN115895297 A CN 115895297A
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Abstract
A preparation method of a modified wollastonite PVC stabilizer comprises the following steps: step one, preparing a crystal seed guiding agent, and mixing sodium metaaluminate, sodium silicate and water according to parts by weight to form the crystal seed guiding agent; secondly, adding kaolin, calcium hydroxide and sodium hydroxide into the seed crystal guiding agent according to parts by weight, stirring and mixing, and carrying out crystallization reaction to obtain a wollastonite PVC stabilizer; and step three, adding a surface modifier into the obtained wollastonite PVC stabilizer to organically modify the surface of the material, wherein the addition amount of the modifier accounts for 0.5-5.0% of the total mass of the wollastonite PVC stabilizer, and after modification, performing pressure filtration, drying and grinding to obtain the modified wollastonite PVC stabilizer. The modified wollastonite PVC stabilizer prepared by the invention has excellent thermal stability, good compatibility with PVC, high product yield, short production period and good continuous production stability.
Description
Technical Field
The invention belongs to the technical field of fine chemical engineering, and particularly relates to a preparation method of a modified wollastonite PVC stabilizer.
Background
Polyvinyl chloride (PVC), one of the earliest resin varieties for industrialization, has good barrier properties, acid and alkali resistance and transparency, and is widely used in the fields of buildings, traffic, offices, lives and the like due to excellent physical and chemical properties. Because the PVC chain contains unstable structures such as allyl chloride and the like, the PVC chain is easy to remove hydrogen chloride and degrade under the action of heat, oxygen, shearing force and the like in the PVC processing process. Therefore, in the processing of PVC, a heat stabilizer and an internal/external lubricant are required to be added for smooth processing. The traditional PVC heat stabilizer generally mainly comprises lead, cadmium and other heavy metals, although the stabilizer has excellent performance, the stabilizer has great harm to human bodies and the environment, along with the development of economy, the living standard of people is improved, the environmental awareness and the health idea are sublimed, and the social requirement on nontoxic and environment-friendly PVC products is stricter and the demand is larger and larger. The modified wollastonite PVC stabilizer belongs to aluminosilicate, has a stable structure, is non-volatile, non-migratory and non-degradable in PVC, has excellent weather resistance, and is an environment-friendly PVC calcium zinc stabilizer with excellent performance. Therefore, how to better prepare the environment-friendly PVC calcium zinc stabilizer becomes the direction of efforts of various manufacturers.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of a modified wollastonite PVC stabilizer.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of a modified wollastonite PVC stabilizer comprises the following steps:
step one, preparing a seed crystal guiding agent, and mixing 15-25 parts of sodium metaaluminate, 10-20 parts of sodium silicate and 70-90 parts of water according to parts by weight to form the seed crystal guiding agent;
step two, adding 30-55 parts of kaolin, 15-30 parts of calcium hydroxide and 2-4 parts of sodium hydroxide into the seed crystal guiding agent according to parts by weight, stirring and mixing, and carrying out crystallization reaction to obtain a wollastonite PVC stabilizer;
and step three, adding a surface modifier into the obtained wollastonite PVC stabilizer to organically modify the surface of the material, wherein the addition amount of the modifier accounts for 0.5-5.0 percent of the total mass of the wollastonite PVC stabilizer, the modification reaction time is 60-150 min, and after the modification is finished, performing filter pressing, drying and grinding to obtain the modified wollastonite PVC stabilizer.
In the first step, after mixing sodium metaaluminate, sodium silicate and water, al is contained in the solution formed 2 O 3 The concentration is 20-150 g/L, siO 2 The content is 5-30%.
In the first step, sodium metaaluminate, sodium silicate and water are mixed, the reaction time is controlled to be 30-80 min, the reaction temperature is 50-150 ℃, and the stirring speed is 100-500 r/min.
In the second step, after sodium hydroxide is added into the seed crystal guiding agent, the sodium hydroxide is used as a sodium source to adjust the ratio of silicon to sodium to be 0.3-2, the pH value is adjusted to be 11.0-12.0 by the sodium hydroxide, the crystallization time is controlled to be 4-15 h, and the crystallization temperature is 50-150 ℃.
The modifier is one or a combination of stearic acid, palmitic acid, lauric acid, glyceryl monostearate, epoxidized soybean oil, pentaerythritol ester, a silane coupling agent, a titanate coupling agent, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, span series and tween series nonionic surfactants.
The sum of the mass of the calcined kaolin and the calcium hydroxide is 1.5 to 2.5 times of the mass of the seed crystal guiding agent.
The preparation method provided by the invention is simple and efficient, has stable process and is easy for industrial production, and the prepared modified wollastonite PVC stabilizer has high yield, excellent thermal stability, excellent dispersibility in PVC and no migration or precipitation.
The modified wollastonite PVC stabilizer prepared by the invention has small particle size, high purity and good continuous production stability, and has better long-term heat resistance to PVC than the traditional aluminosilicate.
Through organic surface modification, the dispersibility of the modified wollastonite in PVC is greatly improved, the agglomeration phenomenon is reduced, and the compatibility with PVC resin is improved.
The modified wollastonite prepared by the invention has wide application prospects in the fields of sewage treatment, heavy metal adsorption, high polymer material acid absorption and the like.
Drawings
FIG. 1 is a schematic XRD spectrum of a sample of a modified wollastonite PVC stabilizer prepared in accordance with the present invention.
Detailed Description
The invention is further illustrated by the following specific examples.
Example 1
Step one, weighing 18.3g of sodium silicate and 11.4g of sodium metaaluminate, adding 500mL of water to prepare slurry, pouring the slurry into a closed three-neck flask for reaction at the reaction temperature of 80 ℃ for 60min at the stirring speed of 300r/min, and preparing the seed crystal guiding agent.
And step two, adding 40g of kaolin, 20g of calcium hydroxide and 2.3g of sodium hydroxide into the prepared seed crystal guiding agent, stirring for 30min, and then controlling the temperature to be 90 ℃ for constant-temperature crystallization for 8h to obtain the wollastonite PVC stabilizer.
And step three, adding 5g of stearic acid into the prepared wollastonite PVC stabilizer in the step two, stirring, modifying for 1h, and then performing filter pressing, drying and grinding to obtain the modified wollastonite PVC stabilizer.
Example 2
Step one, weighing 18.3g of sodium silicate and 11.4g of sodium metaaluminate, adding 500mL of water to prepare slurry, pouring the slurry into a closed three-neck flask for reaction at the reaction temperature of 90 ℃ for 60min at the stirring speed of 300r/min, and preparing the seed crystal guiding agent.
And step two, adding 40g of kaolin, 20g of calcium hydroxide and 2.3g of sodium hydroxide into the prepared seed crystal guiding agent, stirring for 30min, and then controlling the temperature to be 100 ℃ for constant-temperature crystallization for 8h to obtain the wollastonite PVC stabilizer.
And step three, adding 5g of palmitic acid into the wollastonite PVC stabilizer prepared in the step two, starting stirring, modifying for 1h, and then performing filter pressing, drying and grinding to obtain the modified wollastonite PVC stabilizer.
Example 3
Step one, weighing 18.3g of sodium silicate and 11.4g of sodium metaaluminate, adding 500mL of water to prepare slurry, pouring the slurry into a closed three-neck flask for reaction at the reaction temperature of 100 ℃ for 60min at the stirring speed of 300r/min, and preparing the seed crystal guiding agent.
And step two, adding 40g of kaolin, 20g of calcium hydroxide and 2.3g of sodium hydroxide into the prepared seed crystal guiding agent, stirring for 30min, and then controlling the temperature to be 110 ℃ for constant-temperature crystallization for 10h to obtain the wollastonite PVC stabilizer.
And step three, adding 5g of silane coupling agent into the wollastonite PVC stabilizer prepared in the step two, starting stirring, modifying for 1h, and then carrying out filter pressing, drying and grinding to obtain the modified wollastonite PVC stabilizer.
Example 4
Step one, weighing 36.6g of sodium silicate and 22.8g of sodium metaaluminate, adding 1000mL of water to prepare slurry, pouring the slurry into a closed three-neck flask for reaction at the reaction temperature of 100 ℃ for 60min at the stirring speed of 300r/min, and preparing the seed crystal guiding agent.
And step two, adding 80g of kaolin, 40g of calcium hydroxide and 4.6g of sodium hydroxide into the prepared seed crystal guiding agent, stirring for 30min, and then controlling the temperature to be 110 ℃ for constant-temperature crystallization for 10h to obtain the wollastonite PVC stabilizer.
And step three, adding 10g of glyceryl monostearate into the wollastonite PVC stabilizer prepared in the step two, starting stirring, modifying for 1h, and then carrying out filter pressing, drying and grinding to obtain the modified wollastonite PVC stabilizer.
The particle size of the modified wollastonite PVC stabilizer prepared in the examples and the particle size of the conventional zeolite stabilizer were measured by a laser particle sizer, and the measurement results are shown in table 1. Compared with the zeolite of the comparative example, the modified wollastonite PVC stabilizer prepared by the invention has small particle size and is not easy to agglomerate.
TABLE 1
| Detecting items | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example |
| Particle size μm (D50) | 8.5 | 8.6 | 8.5 | 8.8 | 10.5 |
The modified wollastonite PVC stabilizer prepared in the example is applied to PVC to detect the difference between the thermal stability and the traditional zeolite, and the pelleting detection result is shown in Table 2. The result of the table 2 shows that the initial and long-term thermal stability of the modified wollastonite PVC stabilizer prepared by the invention is superior to that of a zeolite stabilizer.
TABLE 2
The acid absorption of the wollastonite PVC stabilizer prepared in the embodiment is detected by applying the wollastonite PVC stabilizer in PVC, the detection mode refers to national standard GB/T2917.1-2002, the detection result is shown in Table 3, and the color change time in Congo red test is long, which indicates that the modified wollastonite PVC stabilizer has higher acid absorption capability than the traditional zeolite material.
TABLE 3
| Sample (I) | Time to change color (min) |
| Example 1 | 62 |
| Example 1 | 65 |
| Example 1 | 63 |
| Example 1 | 64 |
| Comparative example | 58 |
XRD radiation examination of the modified wollastonite PVC stabilizer prepared in the examples was carried out, and as shown in FIG. 1, the XRD pattern of the prepared modified wollastonite PVC stabilizer sample was obtained.
From the above test data, it can be seen that the modified wollastonite PVC stabilizer prepared by the present invention is superior to the conventional zeolite stabilizer.
Although the present invention has been described in detail with reference to the embodiments, it will be apparent to those skilled in the art that modifications, equivalents, improvements, and the like can be made in the technical solutions of the foregoing embodiments or in some of the technical features of the foregoing embodiments, but those modifications, equivalents, improvements, and the like are all within the spirit and principle of the present invention.
Claims (6)
1. A preparation method of a modified wollastonite PVC stabilizer is characterized by comprising the following steps:
step one, preparing a seed crystal guiding agent, and mixing 15-25 parts of sodium metaaluminate, 10-20 parts of sodium silicate and 70-90 parts of water according to parts by weight to form the seed crystal guiding agent;
step two, adding 30-55 parts of kaolin, 15-30 parts of calcium hydroxide and 2-4 parts of sodium hydroxide into the seed crystal guiding agent according to parts by weight, stirring and mixing, and carrying out crystallization reaction to obtain a wollastonite PVC stabilizer;
and step three, adding a surface modifier into the obtained wollastonite PVC stabilizer to organically modify the surface of the material, wherein the addition amount of the modifier accounts for 0.5-5.0% of the total mass of the wollastonite PVC stabilizer, the modification reaction time is 60-150 min, and after the modification is finished, performing filter pressing, drying and grinding to obtain the modified wollastonite PVC stabilizer.
2. The process for preparing a modified wollastonite PVC stabilizer as set forth in claim 1, wherein in the first step, the solution formed by mixing sodium metaaluminate, natron and water contains Al 2 O 3 The concentration is 20-150 g/L, siO 2 The content is 5-30%.
3. The method for preparing the modified wollastonite PVC stabilizer according to claim 2, wherein in the first step, after mixing sodium metaaluminate, sodium silicate and water, the reaction time is controlled to be 30-80 min, the reaction temperature is controlled to be 50-150 ℃, and the stirring speed is controlled to be 100-500 r/min.
4. The method for preparing the modified wollastonite PVC stabilizer according to claim 1, wherein in the second step, after the sodium hydroxide is added into the seed crystal guiding agent, the sodium hydroxide is used as a sodium source to adjust the silica-sodium ratio to be 0.3-2, the pH is adjusted to be 11.0-12.0 by the sodium hydroxide, the crystallization time is controlled to be 4-15 h, and the crystallization temperature is 50-150 ℃.
5. The method of claim 1, wherein the modifier is one or more selected from stearic acid, palmitic acid, lauric acid, glyceryl monostearate, epoxidized soybean oil, pentaerythritol ester, silane coupling agents, titanate coupling agents, sodium dodecylbenzenesulfonate, sodium dodecylsulfate, sodium dodecylsulfonate, span series and tween series nonionic surfactants.
6. The process for preparing a modified canasite PVC stabilizer according to claim 1, wherein the sum of the mass of the calcined kaolin and the calcium hydroxide is 1.5-2.5 times the mass of the seed crystal director.
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| US5139760A (en) * | 1989-02-28 | 1992-08-18 | Mizusawa Industrial Chemicals, Ltd. | Amorphous silica-alumina spherical particles and process for preparation thereof |
| CN1285806A (en) * | 1997-10-31 | 2001-02-28 | 花王株式会社 | Aluminoshilicate |
| CN1365375A (en) * | 1999-07-29 | 2002-08-21 | Pq控股公司 | Aluminosilicates stabilized halogenated polymers |
| CN102000604A (en) * | 2010-10-12 | 2011-04-06 | 江苏大学 | Method for synthesizing composite molecular sieve by microwave method and catalytic performance application thereof |
| CN104150518A (en) * | 2014-08-05 | 2014-11-19 | 邵阳天堂助剂化工有限公司 | Synthesis method for hydrocalumites and hydrocalumites based PVC complex heat stabilizer |
| CN108395643A (en) * | 2018-03-23 | 2018-08-14 | 邵阳学院 | Modification hydrocalumite and its clean method for preparing for PVC heat stabilizer |
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- 2022-12-20 CN CN202211640772.2A patent/CN115895297A/en active Pending
Patent Citations (8)
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| US5139760A (en) * | 1989-02-28 | 1992-08-18 | Mizusawa Industrial Chemicals, Ltd. | Amorphous silica-alumina spherical particles and process for preparation thereof |
| US4976786A (en) * | 1989-10-04 | 1990-12-11 | Ecc America Inc. | Method for forming aggregated kaolin pigment |
| CN1285806A (en) * | 1997-10-31 | 2001-02-28 | 花王株式会社 | Aluminoshilicate |
| CN1365375A (en) * | 1999-07-29 | 2002-08-21 | Pq控股公司 | Aluminosilicates stabilized halogenated polymers |
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| CN108623843A (en) * | 2018-03-23 | 2018-10-09 | 邵阳天堂助剂化工有限公司 | Modified hydrotalcite and its clean method for preparing for PVC heat stabilizer |
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