CN112540146A - Method for evaluating organic surface coating effect of special titanium dioxide for plastics - Google Patents

Method for evaluating organic surface coating effect of special titanium dioxide for plastics Download PDF

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Publication number
CN112540146A
CN112540146A CN201910893280.6A CN201910893280A CN112540146A CN 112540146 A CN112540146 A CN 112540146A CN 201910893280 A CN201910893280 A CN 201910893280A CN 112540146 A CN112540146 A CN 112540146A
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titanium dioxide
surface coating
organic surface
coating effect
special
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Chinese (zh)
Inventor
肖勇丽
景建林
赵北东
和柳
李开娟
徐庭敏
周俊
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Chongqing Titanium Industry Co Ltd of Pangang Group
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Chongqing Titanium Industry Co Ltd of Pangang Group
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N5/00Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
    • G01N5/04Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder

Abstract

The invention belongs to the technical field of chemical industry, and particularly relates to a method for evaluating the organic surface coating effect of special titanium dioxide for plastics. The invention aims to solve the technical problem of providing a method for evaluating the organic surface coating effect of special titanium dioxide for plastics. The method comprises the following steps: A. drying the titanium dioxide, cooling to room temperature, adding the titanium dioxide into desalted water, stirring, and observing and recording the hydrophobic condition of the titanium dioxide; B. heating the desalted water containing titanium dioxide in the step A, carrying out condensation reflux in the heating process, cooling after heating is finished, and filtering to obtain filtrate and residues; C. the residue was calcined, cooled and weighed, and the filtrate was subjected to turbidity measurement. The method can quantitatively and accurately evaluate the organic surface coating effect of the titanium dioxide special for different plastics.

Description

Method for evaluating organic surface coating effect of special titanium dioxide for plastics
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a method for evaluating the organic surface coating effect of special titanium dioxide for plastics.
Background
Titanium dioxide (titanium dioxide, a scientific name) is the best white pigment in the world at present, not only has very stable physical and chemical properties, but also has excellent optical and electrical properties such as high refractive index, optimal covering power, optimal whiteness and brightness, and the like, is widely applied to the fields of coatings, plastics, papermaking, printing ink, electronics and the like, and is called as industrial monosodium glutamate.
The plastic industry is the second largest user of titanium dioxide, the development is rapid in recent years, and about 25% of titanium dioxide yield is applied to the plastic industry. Many plastic products are based on synthetic resins and contain fillers, colorants, plasticizers, and the like. Colorants play a critical role in coloring plastics. There are many methods for coloring plastics, and color masterbatch coloring is the most commonly used method for coloring plastics. The color master batch is a special coloring agent for novel high molecular materials, also called pigment preparation, which consists of three basic elements of pigment or dye, carrier and additive, and is an aggregate obtained by uniformly loading an excessive amount of pigment or dye into resin, which can be called pigment concentrate, so that the coloring power of the color master batch is higher than that of the pigment per se. Therefore, the coloring of plastic articles is usually carried out by making pigments into color concentrates. The titanium dioxide particles contain polar groups on the surfaces, are easy to wet by water, are difficult to wet and disperse in non-polar media such as plastics, color masterbatch and the like, and need to be subjected to organic surface coating treatment in order to improve the compatibility of the titanium dioxide pigment particles and a resin system and improve the dispersion performance of the titanium dioxide pigment particles in the plastics and the color masterbatch system. At present, the special titanium dioxide for plastics at home and abroad is subjected to organic surface coating treatment.
The organic surface coating treatment mode of titanium dioxide mainly comprises two treatment modes, namely physical adsorption and chemical adsorption. The organic active agent molecule is generally composed of two parts of hydrophilic polar group and oleophilic non-polar group, when it contacts with polar titanium dioxide molecule, its polar group is adsorbed on the surface of titanium dioxide, or it is chemically bonded with polar group on the surface of titanium dioxide granule, and partial branched chains of organic treating agent are chemically bonded with each other, so that the titanium dioxide granule is completely covered, and partial branched chains whose tail end is non-polar group are compatible with resin, so that the titanium dioxide is completely hydrophobic and oleophilic, and can attain the goal of raising compatibility with resin system and improving dispersibility in soft plastic system. The better the coating effect of the organic surface of the special titanium dioxide for plastics is, the poorer the compatibility of the titanium dioxide with water is, and the lower the turbidity of the filtered water solution is.
Patent CN105259130A discloses a method for detecting the stability of organic treatment on the surface of titanium dioxide, which adopts an infrared spectrometer to detect the difference of energy spectrums before and after the titanium dioxide is added with an organic treatment agent, thereby analyzing and judging the stability of the addition amount of the organic treatment agent. The method can only be used for analyzing the stability of the adding amount of the titanium dioxide organic treating agent, and the method cannot be used for judging the coating effect of the titanium dioxide organic surface.
Disclosure of Invention
The invention aims to provide a method for evaluating the organic surface coating effect of special titanium dioxide for plastics.
The invention provides a method for evaluating the organic surface coating effect of special plastic titanium dioxide, which comprises the following steps:
A. drying the titanium dioxide, cooling to room temperature, adding the titanium dioxide into desalted water, stirring, and observing and recording the hydrophobic condition of the titanium dioxide;
B. heating the desalted water containing titanium dioxide in the step A, carrying out condensation reflux in the heating process, cooling after heating is finished, and filtering to obtain filtrate and residues;
C. the residue was calcined, cooled and weighed, and the filtrate was subjected to turbidity measurement.
Further, in the step A, the drying condition of the titanium dioxide is to keep the temperature at 105 ℃ for 1-4 h.
Further, in the step A, the titanium dioxide is added into desalted water according to the weight ratio of 1 g: 100mL of the solution was added.
Further, in the step B, a temperature-controllable electric heating plate is adopted for heating, the heating temperature is 120-180 ℃, and the heating time is 10-25 min.
Further, in the step B, the filtration is carried out by adopting quantitative filter paper.
Further, in step C, the residue is calcined at 850 ℃ for 1-3 h.
Further, in the step C, the turbidity measurement is performed by any one of spectrophotometry, visual turbidimetry, and turbidimetric measurement.
The invention has the beneficial effects that:
the method can quantitatively and accurately evaluate the organic surface coating effect of the special titanium dioxide for plastics, can help plastic color master customers to select the special titanium dioxide for plastics, and provides guidance for evaluating the organic surface treatment effect of titanium dioxide production of plastic color master special titanium dioxide manufacturers. The method can accurately and quantitatively judge and evaluate the organic coating effect of the titanium dioxide for plastics of different grades.
Detailed Description
The raw materials and equipment used in the embodiment of the present invention are known products and obtained by purchasing commercially available products.
Specifically, the invention provides a method for evaluating the organic surface coating effect of the special titanium dioxide for plastics. The method comprises the following steps:
A. drying the titanium dioxide, cooling to room temperature, adding the titanium dioxide into desalted water, stirring, and observing and recording the hydrophobic condition of the titanium dioxide;
B. heating the desalted water containing titanium dioxide in the step A, carrying out condensation reflux in the heating process, cooling after heating is finished, and filtering to obtain filtrate and residues;
C. the residue was calcined, cooled and weighed, and the filtrate was subjected to turbidity measurement.
In the step A of the invention, in order to avoid the interference of moisture and ensure the accuracy of the measurement result, the special titanium dioxide for plastics is dried firstly, the temperature is kept at 105 ℃ for 1-4h, the dried titanium dioxide is cooled to the room temperature, and the weight ratio of the titanium dioxide to the water is 1 g: adding 100mL of the titanium pigment into desalted water, stirring, and observing and recording the hydrophobic condition of the titanium pigment. Hydrophobic refers to the ability of a product to resist the adverse effects of environmental moisture on its primary properties. If the titanium dioxide can completely float on the water surface and is completely incompatible with water, the titanium dioxide is completely hydrophobic, which indicates that the titanium dioxide is completely coated by the organic treating agent; the partial hydrophobicity shows that the titanium dioxide powder is partially coated by the organic treating agent.
In the step B of the invention, the desalted water containing titanium dioxide in the step A is heated to destroy the organic surface coating of the titanium dioxide, preferably, an electric heating plate is adopted for heating to ensure that the sample is heated uniformly and stably, a condensation reflux device is arranged in the heating process to avoid the volatilization of liquid and improve the accuracy of the measurement result. Heating at 120-180 deg.C for 10-25min, cooling to room temperature, and filtering with quantitative filter paper to obtain filtrate and residue.
In step C of the invention, the residue is calcined, and the residue can be transferred into a clean crucible, put into a muffle furnace and calcined to constant weight, and the weight of the residue is accurately weighed. The filtrate is subjected to turbidity measurement by any one of spectrophotometry, visual turbidimetry or turbidimetry. The higher the weight of the residue, the lower the turbidity of the filtrate, indicating that the titanium dioxide has the better organic surface coating effect.
The present invention will be further illustrated by the following specific examples.
The plastic-dedicated titanium dioxide powders used in the following examples were purchased from different manufacturers, and defined as a brand a, a brand B, and a brand C, respectively, and subjected to surface coating effect evaluation.
Example 1
10g (to the nearest 0.01g) of the special plastic titanium dioxide A is weighed into a weighing bottle, dried in an oven at 105 ℃ for 2 hours, covered and placed in a drying dish to be cooled to room temperature. A500 mL dry Erlenmeyer flask was prepared, and 200mL of desalted water was accurately measured and poured into the Erlenmeyer flask. Accurately weighing 2g (accurate to 0.0001g) of the titanium dioxide, quantitatively transferring the titanium dioxide into a 500mL conical flask, stirring, observing and recording the hydrophobic condition of the titanium dioxide, and installing a condensation reflux device at the opening of the conical flask. The conical flask is moved to an electric heating plate, a power switch of the electric heating plate is turned on, the heating temperature is set to be 150 ℃, and heating is carried out for 15 minutes. And (5) turning off the power supply of the electric heating plate, and cooling to room temperature. Filtering the solution in the conical flask with quantitative filter paper, transferring the filter paper and the residue on the filter paper into a clean crucible, calcining in a muffle furnace at 850 deg.C for 1 hr, covering, cooling to room temperature in a drying dish, and accurately weighing the residue to obtain a weight Ga1(ii) a The filtrate adopts visual ratioTurbidity was measured by the turbidity method.
Example 2
10g (to the nearest 0.01g) of the special plastic titanium dioxide B is weighed into a weighing bottle, dried in an oven at 105 ℃ for 3 hours, covered and placed in a drying dish to be cooled to room temperature. A500 mL dry Erlenmeyer flask was prepared, and 200mL of desalted water was accurately measured and poured into the Erlenmeyer flask. Accurately weighing 2g (accurate to 0.0001g) of the titanium dioxide, quantitatively transferring the titanium dioxide into a 500mL conical flask, stirring, observing and recording the hydrophobic condition of the titanium dioxide, and installing a condensation reflux device at the opening of the conical flask. The conical flask is moved to an electric heating plate, a power switch of the electric heating plate is turned on, the heating temperature is set to be 150 ℃, and heating is carried out for 15 minutes. And (5) turning off the power supply of the electric heating plate, and cooling to room temperature. Filtering the solution in the conical flask with quantitative filter paper, transferring the filter paper and the residue on the filter paper into a clean crucible, calcining in a muffle furnace at 850 deg.C for 3 hr, covering, cooling to room temperature in a drying dish, and accurately weighing the residue to obtain a weight Gb1(ii) a The filtrate was measured for turbidity by visual turbidimetry.
Example 3
10g (exactly to 0.01g) of the special plastic titanium dioxide C is weighed into a weighing bottle, dried in an oven at 105 ℃ for 4 hours, covered and placed in a drying dish to be cooled to room temperature. A500 mL dry Erlenmeyer flask was prepared, and 200mL of desalted water was accurately measured and poured into the Erlenmeyer flask. Accurately weighing 2g (accurate to 0.0001g) of the titanium dioxide, quantitatively transferring the titanium dioxide into a 500mL conical flask, stirring, observing and recording the hydrophobic condition of the titanium dioxide, and installing a condensation reflux device at the opening of the conical flask. The conical flask is moved to an electric heating plate, a power switch of the electric heating plate is turned on, the heating temperature is set to be 150 ℃, and heating is carried out for 15 minutes. And (5) turning off the power supply of the electric heating plate, and cooling to room temperature. Filtering the solution in the conical flask with quantitative filter paper, transferring the filter paper and the residue on the filter paper into a clean crucible, calcining in a muffle furnace at 850 deg.C for 2 hr, covering, cooling to room temperature in a drying dish, and accurately weighing the residue to obtain a weight Gc1(ii) a The filtrate was measured for turbidity by visual turbidimetry.
Example 4
Weighing 10g (accurate to 0.01g) of special plastic titanium dioxide C in a weighing bottle, and drying in an ovenDried at 105 ℃ for 1 hour, covered and placed in a drying dish to cool to room temperature. A500 mL dry Erlenmeyer flask was prepared, and 200mL of desalted water was accurately measured and poured into the Erlenmeyer flask. Accurately weighing 2g (accurate to 0.0001g) of the titanium dioxide, quantitatively transferring the titanium dioxide into a 500mL conical flask, stirring, observing and recording the hydrophobic condition of the titanium dioxide, and installing a condensation reflux device at the opening of the conical flask. The conical flask is moved to an electric heating plate, a power switch of the electric heating plate is turned on, the heating temperature is set to be 120 ℃, and the conical flask is heated for 10 minutes. And (5) turning off the power supply of the electric heating plate, and cooling to room temperature. Filtering the solution in the conical flask with quantitative filter paper, transferring the filter paper and the residue on the filter paper into a clean crucible, calcining in a muffle furnace at 850 deg.C for 1 hr, covering, cooling to room temperature in a drying dish, and accurately weighing the residue to obtain a weight Gc1(ii) a The filtrate was measured for turbidity by visual turbidimetry.
Example 5
10g (exactly to 0.01g) of the special plastic titanium dioxide C is weighed into a weighing bottle, dried in an oven at 105 ℃ for 4 hours, covered and placed in a drying dish to be cooled to room temperature. A500 mL dry Erlenmeyer flask was prepared, and 200mL of desalted water was accurately measured and poured into the Erlenmeyer flask. Accurately weighing 2g (accurate to 0.0001g) of the titanium dioxide, quantitatively transferring the titanium dioxide into a 500mL conical flask, stirring, observing and recording the hydrophobic condition of the titanium dioxide, and installing a condensation reflux device at the opening of the conical flask. The conical flask is moved to an electric heating plate, a power switch of the electric heating plate is turned on, the heating temperature is set to be 180 ℃, and heating is carried out for 25 minutes. And (5) turning off the power supply of the electric heating plate, and cooling to room temperature. Filtering the solution in the conical flask with quantitative filter paper, transferring the filter paper and the residue on the filter paper into a clean crucible, calcining in a muffle furnace at 850 deg.C for 2 hr, covering, cooling to room temperature in a drying dish, and accurately weighing the residue to obtain a weight Gc1(ii) a The filtrate was measured for turbidity by visual turbidimetry. The hydrophobicity of the samples of examples 1-5, the weight of the residue obtained and the turbidity of the filtrate are shown in Table 1.
TABLE 1 evaluation results of organic coating effect of samples of different brands
Figure BDA0002209444100000041
As can be seen from examples 1-5, the organic surface coating effect of the titanium dioxide A, B, C special for plastic is B > C > A. The method can quantitatively and accurately evaluate the organic surface coating effect of the titanium dioxide special for different plastics. The method can help plastic color master customers to select the special plastic titanium dioxide, and provides guidance for evaluating the organic surface treatment effect of titanium dioxide production of plastic color master special titanium dioxide manufacturers.

Claims (7)

1. The method for evaluating the organic surface coating effect of the special plastic titanium dioxide is characterized by comprising the following steps: the method comprises the following steps:
A. drying the titanium dioxide, cooling to room temperature, adding the titanium dioxide into desalted water, stirring, and observing and recording the hydrophobic condition of the titanium dioxide;
B. heating the desalted water containing titanium dioxide in the step A, carrying out condensation reflux in the heating process, cooling after heating is finished, and filtering to obtain filtrate and residues;
C. the residue was calcined, cooled and weighed, and the filtrate was subjected to turbidity measurement.
2. The method for evaluating the organic surface coating effect of the special titanium dioxide for plastics according to claim 1, which is characterized in that: in the step A, the drying condition of the titanium dioxide is to keep the temperature at 105 ℃ for 1-4 h.
3. The method for evaluating the organic surface coating effect of the special titanium dioxide for plastics according to claim 1 or 2, which is characterized in that: in the step A, adding the titanium dioxide into desalted water according to the weight ratio of 1 g: 100mL of the solution was added.
4. The method for evaluating the organic surface coating effect of the special titanium dioxide for plastics according to any one of claims 1 to 3, wherein the method comprises the following steps: in the step B, the heating adopts a temperature-controllable electric heating plate, the heating temperature is 120-180 ℃, and the heating time is 10-25 min.
5. The method for evaluating the organic surface coating effect of the special titanium dioxide for plastics according to any one of claims 1 to 4, wherein: and in the step B, filtering by adopting quantitative filter paper.
6. The method for evaluating the organic surface coating effect of the special titanium dioxide for plastics according to any one of claims 1 to 5, wherein: in step C, the residue is calcined at 850 ℃ for 1-3 h.
7. The method for evaluating the organic surface coating effect of the special titanium dioxide for plastics according to any one of claims 1 to 6, wherein: in step C, the turbidity is measured by any one of spectrophotometry, visual turbidimetry or turbidimetry.
CN201910893280.6A 2019-09-20 2019-09-20 Method for evaluating organic surface coating effect of special titanium dioxide for plastics Pending CN112540146A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113252497A (en) * 2021-05-12 2021-08-13 攀钢集团重庆钒钛科技有限公司 Method for detecting uniformity of organic coating of titanium dioxide special for plastics

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113252497A (en) * 2021-05-12 2021-08-13 攀钢集团重庆钒钛科技有限公司 Method for detecting uniformity of organic coating of titanium dioxide special for plastics

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