CN107941584B - Performance test method of modified activated calcium carbonate - Google Patents
Performance test method of modified activated calcium carbonate Download PDFInfo
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- CN107941584B CN107941584B CN201711295485.1A CN201711295485A CN107941584B CN 107941584 B CN107941584 B CN 107941584B CN 201711295485 A CN201711295485 A CN 201711295485A CN 107941584 B CN107941584 B CN 107941584B
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a performance test method of modified activated calcium carbonate. Relates to the technical field of modified calcium carbonate detection. The method comprises the steps of preparing a sample and analyzing the sample, namely adding different amounts of coupling agents into 10kg of calcium carbonate emulsion respectively, grouping, filtering and washing the mixture while the mixture is hot, removing unreacted coupling agents, drying and grinding the mixture to obtain active calcium carbonate powder; separately selecting calcium carbonate powder without activation treatment for grouping, selecting absolute ethyl alcohol as extraction liquid, adding the modified calcium carbonate and the unmodified calcium carbonate into polyvinyl chloride resin according to the proportion of 30 percent, preparing a sample strip, and testing the mechanical property of the sample strip. The invention takes the absolute ethyl alcohol as the extracting agent, the absolute ethyl alcohol is easy to prepare, the cost of the experiment is effectively reduced, the sample strips are prepared by mixing the calcium carbonate powder and the polyvinyl chloride resin, the experimental data is obtained by the verification of experimental equipment, the experimental process is simple and easy to operate, and the experimental error is reduced.
Description
Technical Field
The invention belongs to the technical field of modified calcium carbonate detection, and particularly relates to a performance test method of modified activated calcium carbonate.
Background
The active calcium carbonate is used as high-grade filler with high filling amount, and is widely applied to industries such as rubber, plastics, plastic-steel doors and windows, PVC cable materials, high-grade coatings, pipes, tires, soles, polyethylene blown films, sealing rubber strips, glass fiber reinforced plastic products, cable packaging cloth, papermaking, building materials, printing ink, daily chemical industry, textiles, feeds, food additives and the like.
The active calcium carbonate is used as a base material, and is prepared by modifying and activating the surface of inorganic powder by adopting a multifunctional surfactant and a composite efficient processing aid. The modified calcium carbonate powder has one special coating structure formed on its surface, and can improve the dispersivity and affinity in polyolefin polymer matrix and produce interface effect with the polymer matrix to raise the shock strength of the product. The filling amount is generally 30-100%, and some products are even more than 100 parts. The existing detection process of modified calcium carbonate is complicated, the data processing capacity of the experiment is large, and the experimental deviation is easy to cause.
Disclosure of Invention
The invention aims to provide a performance testing method of modified activated calcium carbonate, which uses absolute ethyl alcohol as an extracting agent, wherein the absolute ethyl alcohol is easy to prepare, so that the experimental cost is effectively reduced, and the experimental data is obtained through the verification of experimental equipment by mixing calcium carbonate powder with polyvinyl chloride resin to prepare sample strips, so that the experimental process is simple and convenient and easy to operate, and the experimental error is reduced.
In order to solve the technical problems, the invention is realized by the following technical scheme:
the invention relates to a performance test method of modified activated calcium carbonate, which comprises the following steps:
step one, manufacturing a sample: adding 10kg of calcium carbonate emulsion into a high-speed mixer, heating to 120 ℃, adding coupling agents with the amount of 1%, 2%, 3% and 4% of the mass of calcium carbonate respectively, numbering samples with the numbers of No. 1, No. 2, No. 3 and No. 4 respectively, activating for 8min, filtering and washing while hot, removing unreacted coupling agents, drying and grinding to obtain active calcium carbonate powder;
step two, sample analysis: selecting calcium carbonate powder with the serial number of No. 5 without activation treatment, taking a sample with the mass of M and untreated calcium carbonate with the mass of M, respectively placing the samples and the untreated calcium carbonate into different volumetric barrels,
a, selecting absolute ethyl alcohol as extraction liquid, taking the boiling point of the absolute ethyl alcohol and the performance of a coupling agent into consideration, selecting the temperature to be 20-50 ℃, the time to be 30-120min, washing and drying after the extraction is finished, and then weighing the mass M1And then the mass after drying is M1The sample is calcined at 450 ℃ for 1h and cooled to obtain a mass M2The extraction grafting ratio gamma is M1-M2/M-M1；
b, adding the modified calcium carbonate and the unmodified calcium carbonate into the polyvinyl chloride resin according to the proportion of 30 percent to prepare a sample strip, and testing the mechanical property of the sample strip.
Further, the rotating speed of the medium-high mixer in the first step is fixed at 1400 r/min.
Further, in the second step, the required instruments and devices comprise a balance, a volumetric cylinder, a ruler and a small shovel.
Further, in the substep a in the second step, the extraction temperature is 20 ℃, 35 ℃ and 50 ℃, and the extraction time is 30min, 60min, 90min and 120 min.
Further, the mechanical properties tested in the sub-step b in the second step comprise tensile strength, bending strength, impact strength and elongation.
The invention has the following beneficial effects:
the invention takes the absolute ethyl alcohol as the extracting agent, the absolute ethyl alcohol is easy to prepare, the cost of the experiment is effectively reduced, the sample strips are prepared by mixing the calcium carbonate powder and the polyvinyl chloride resin, the experimental data is obtained by the verification of experimental equipment, the experimental process is simple and convenient, the operation is easy, the experimental error is reduced, the experimental result is obtained by a plurality of experiments, and the accuracy of the experimental result is improved.
Of course, it is not necessary for any product in which the invention is practiced to achieve all of the above-described advantages at the same time.
Detailed Description
Technical solutions in the embodiments of the present invention are clearly and completely described, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention relates to a performance test method of modified activated calcium carbonate, which comprises the following steps:
preparation of a sample: adding 10kg of calcium carbonate emulsion into a high-speed mixer, heating to 120 ℃, adding coupling agents with the amount of 1%, 2%, 3% and 4% of the mass of calcium carbonate respectively, numbering samples with the numbers of No. 1, No. 2, No. 3 and No. 4 respectively, activating for 8min, filtering and washing while hot, removing unreacted coupling agents, drying and grinding to obtain active calcium carbonate powder;
and (3) sample analysis: selecting calcium carbonate powder with the serial number of No. 5 without activation treatment, taking a sample with the mass of M and untreated calcium carbonate with the mass of M, respectively placing the samples and the untreated calcium carbonate into different volumetric barrels,
example 1:
selecting anhydrous ethanol as extractive solution, considering anhydrous ethanol boiling point and coupling agent performance, extracting for 30min, and setting three groups of experimental groups at experimental temperatures of 20 deg.C, 35 deg.C and 50 deg.C, respectively, washing and drying after extraction to obtain M1And then the mass after drying is M1The sample is calcined at 450 ℃ for 1h and cooled to obtain a mass M2The extraction grafting ratio gamma is M1-M2/M-M1。
Example 2:
selecting anhydrous ethanol as extractive solution, considering anhydrous ethanol boiling point and coupling agent performance, extracting for 60min, and setting three groups of experimental groups at experimental temperatures of 20 deg.C, 35 deg.C and 50 deg.C, respectively, washing and drying after extraction to obtain M1And then the mass after drying is M1The sample is calcined at 450 ℃ for 1h and cooled to obtain a mass M2The extraction grafting ratio gamma is M1-M2/M-M1。
Example 3:
selecting anhydrous ethanol as extractive solution, considering anhydrous ethanol boiling point and coupling agent performance, extracting for 90min, and setting three groups of experimental groups at experiment temperatures of 20 deg.C, 35 deg.C and 50 deg.C, respectively, washing and drying after extraction to obtain M1And then the mass after drying is M1The sample is calcined at 450 ℃ for 1h and cooled to obtain a mass M2The extraction grafting ratio gamma is M1-M2/M-M1。
Example 4:
selecting anhydrous ethanol as extractive solution, considering anhydrous ethanol boiling point and coupling agent performance, extracting for 120min, and setting three groups of experimental groups at experimental temperatures of 20 deg.C, 35 deg.C and 50 deg.C, respectively, washing and drying after extraction to obtain M1And then the mass after drying is M1The sample is calcined at 450 ℃ for 1h and cooled to obtain a mass M2Extractive graftingRate γ ═ M1-M2/M-M1The amount of coupling agent consumed by extraction is shown in Table 1.
TABLE 1
Example 5
Calcium carbonate powders numbered 1, 2, 3, 4 and 5 were added to polyvinyl chloride resin in a proportion of 30% to prepare sample bars, and the mechanical properties thereof were tested as shown in table 2.
TABLE 2
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (5)
1. A performance test method of modified activated calcium carbonate is characterized by comprising the following steps:
step one, manufacturing a sample: adding 10kg of calcium carbonate emulsion into a high-speed mixer, heating to 120 ℃, adding coupling agents with the amount of 1%, 2%, 3% and 4% of the mass of calcium carbonate respectively, numbering samples with the numbers of No. 1, No. 2, No. 3 and No. 4 respectively, activating for 8min, filtering and washing while hot, removing unreacted coupling agents, drying and grinding to obtain active calcium carbonate powder;
step two, sample analysis: selecting calcium carbonate powder with the serial number of No. 5 without activation treatment, taking a sample with the mass of M and untreated calcium carbonate with the mass of M, respectively placing the samples and the untreated calcium carbonate into different volumetric barrels,
a, selecting absolute ethyl alcohol as extraction liquid, taking the boiling point of the absolute ethyl alcohol and the performance of a coupling agent into consideration, selecting the temperature to be 20-50 ℃, the time to be 30-120min, washing and drying after the extraction is finished, and then weighing the mass M1And then the mass after drying is M1The sample is calcined at 450 ℃ for 1h and cooled to obtain a mass M2The extraction grafting ratio gamma is M1-M2/M-M1；
b, adding the modified calcium carbonate and the unmodified calcium carbonate into the polyvinyl chloride resin according to the proportion of 30 percent to prepare a sample strip, and testing the mechanical property of the sample strip.
2. The method for testing the performance of modified activated calcium carbonate according to claim 1, wherein the rotation speed of the medium-high mixer in the first step is fixed at 1400 r/min.
3. The method for testing the performance of modified activated calcium carbonate according to claim 1, wherein the instrumentation required in the second step comprises a balance, a volumetric cylinder, a ruler and a spatula.
4. The method for testing the performance of modified activated calcium carbonate according to claim 1, wherein the extraction temperature in the substep a in the second step is 20 ℃, 35 ℃, 50 ℃, and the extraction time is 30min, 60min, 90min, 120 min.
5. The method for testing the performance of modified activated calcium carbonate according to claim 1, wherein the mechanical properties tested in the substep b in the second step comprise tensile strength, bending strength, impact strength and elongation.
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| CN105860587A (en) * | 2016-04-01 | 2016-08-17 | 安徽新涛新材料科技有限公司 | Calcium carbonate powder surface modification equipment |
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| CN102200535A (en) * | 2010-03-26 | 2011-09-28 | 中国石油化工股份有限公司 | Method for testing grafting rate, grafting efficiency, rubber content and grafted rubber content of mass acrylonitrile butadiene styrene (ABS) |
| CN107106043B (en) * | 2015-01-16 | 2020-10-30 | 皇家飞利浦有限公司 | Vertebral body feature identification |
| CN105606486A (en) * | 2016-01-27 | 2016-05-25 | 浙江理工大学 | Testing method for modified nano-silica surface grafting state |
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| JP2004183127A (en) * | 2002-12-02 | 2004-07-02 | Achilles Corp | Modified carbon nanofiber, and resin composition and coating material containing the same |
| CN103382277A (en) * | 2013-07-17 | 2013-11-06 | 建德市钦堂碳酸钙行业研发有限公司 | Composite calcium carbonate modified PVC (polyvinyl chloride) rolling film and preparation method thereof |
| CN104448662A (en) * | 2013-09-18 | 2015-03-25 | 中国石油天然气股份有限公司 | Method for preparing low-smoke and high flame retardant powdered butadiene styrene rubber |
| CN105860587A (en) * | 2016-04-01 | 2016-08-17 | 安徽新涛新材料科技有限公司 | Calcium carbonate powder surface modification equipment |
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Denomination of invention: A Performance Testing Method for Modified Activated Calcium Carbonate Effective date of registration: 20230825 Granted publication date: 20200731 Pledgee: Xuancheng Zhenxuan Financing Guarantee Group Co.,Ltd. Pledgor: ANHUI XINTAO NEW MATERIAL TECHNOLOGY CO.,LTD. Registration number: Y2023980053384 |