CN111363386B - Preparation method of titanium dioxide for delustering chinlon chemical fiber - Google Patents
Preparation method of titanium dioxide for delustering chinlon chemical fiber Download PDFInfo
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3653—Treatment with inorganic compounds
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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- C09C1/3669—Treatment with low-molecular organic compounds
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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- C09C1/3607—Titanium dioxide
- C09C1/3676—Treatment with macro-molecular organic compounds
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
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Abstract
A preparation method of titanium dioxide for delustering chinlon chemical fibers is characterized by comprising the following steps: dispersing pigment-grade anatase titanium dioxide into water slurry, and grinding, diluting and grading to remove large particles; then coating antimony oxide and hydrated zirconium oxide on the surfaces of the titanium dioxide particles; and then pentaerythritol is used for treating the surface of the inorganic coated titanium dioxide particles to obtain the titanium dioxide for delustering the nylon chemical fiber.
Description
Technical Field
The invention relates to a preparation method of titanium dioxide for delustering chinlon chemical fibers.
Background
The existing titanium dioxide for delustring of chinlon chemical fiber is coated by hydrated silicon oxide and hydrated aluminum oxide, and the hydrated silicon oxide and the hydrated aluminum oxide are coated, so that the surface of titanium dioxide is isolated from water and oxygen in the air, the aim is to eliminate the photocatalysis phenomenon of the titanium dioxide, and the coating method has the problems that: firstly, due to the existence of hydrated alumina, the hydrated alumina can be reduced into aluminum by caprolactam, scaling is caused on the surface of a heat exchanger tube array of a prepolymerization tower, the heat exchange effect is influenced, the scaling can automatically fall off to a certain thickness, and the fallen matter enters a product to cause subsequent spinning and yarn breaking, so that great loss is caused. Secondly, due to the existence of hydrated silicon oxide, the hydrated silicon oxide is easily washed by the extraction water and enters an extraction water recovery system, water is continuously evaporated in the extraction water recovery system, the concentration of the hydrated silicon oxide is continuously increased, the hydrated silicon oxide is adsorbed in the tube array of the triple-effect evaporator, the heat exchange effect of the triple-effect evaporator is reduced until the tube array of the triple-effect evaporator is blocked, and the production cannot be continued.
In order to solve the problems, the invention adopts the technical scheme that the surface of a titanium dioxide particle is coated with a layer of antimony oxide which can reduce the photocatalysis phenomenon of the titanium dioxide, and then the surface of the titanium dioxide particle is coated with a layer of hydrous zirconium oxide which can isolate the surface of the titanium dioxide from water and oxygen in the air, so that the photocatalysis phenomenon of the titanium dioxide is eliminated. In order to ensure that the obtained titanium dioxide particles have good dispersibility and few large particles, the surfaces of the titanium dioxide particles coated with inorganic films are treated by pentaerythritol, and the pentaerythritol can prevent the titanium dioxide particles from agglomerating.
Disclosure of Invention
A preparation method of titanium dioxide for delustering chinlon chemical fibers is characterized by comprising the following steps: dispersing pigment-grade anatase titanium dioxide into water slurry, and grinding, diluting and grading to remove large particles; then coating antimony oxide and hydrated zirconium oxide on the surfaces of the titanium dioxide particles; and then pentaerythritol is used for treating the surface of the inorganic coated titanium dioxide particles to obtain the titanium dioxide for delustering the nylon chemical fiber.
The method comprises the steps of dispersing pigment-grade anatase titanium dioxide into water slurry, grinding, diluting and grading to remove large particles, and is characterized in that: dispersing 200 parts by weight of pigment-grade anatase titanium dioxide in 200 parts by weight of deionized water, adding 0.4-0.8 part by weight of sodium polyacrylate dispersant, and dispersing for 30-60 minutes by using a high-speed dispersion machine to prepare slurry; grinding the slurry twice by using a grinder, then transferring the slurry into a stirring kettle, adding 800 parts of deionized water into the slurry for dilution, continuously feeding the diluted slurry into a horizontal spiral discharging centrifugal classifier for classification, removing large-particle materials, and feeding fine-particle materials into the stirring kettle for later use.
The method is characterized in that the surface of the titanium dioxide particles is coated with antimony oxide and hydrous zirconium oxide, and the method comprises the following steps: heating the slurry to 80 ℃, adding 0.8-1.2 parts of antimony trichloride into the slurry under continuous stirring, continuously stirring for 30 minutes, slowly adding 4-6 parts of 10% sodium hydroxide into the slurry, and controlling the adding time to be 3 hours; adding 12-15 parts of zirconium oxychloride octahydrate into the slurry under continuous stirring, continuously stirring for 30 minutes, slowly adding 30-40 parts of 10% sodium hydroxide into the slurry, and controlling the adding time to be 3 hours; stirring is continued for 30 minutes, the slurry is sent into a plate-and-frame filter press for filtration, and the filter cake is washed by deionized water until no chloride ion exists.
The surface of the titanium dioxide particles coated with the inorganic coating is treated by pentaerythritol, and the method is characterized in that: putting the filter cake into a pulping tank, adding 300 parts of deionized water into the filter cake for pulping, adding 0.6-0.8 part of sodium polyacrylate dispersant into the pulp, stirring for 30 minutes, weighing 0.5-1.0 part of pentaerythritol, adding the pentaerythritol into the pulp, and stirring for 1 hour to obtain the TiO with the surface modified by the pentaerythritol and uniformly dispersed2And (3) sizing agent, drying the sizing agent, crushing the dried material by using a crusher, and packaging to obtain the titanium dioxide for the nylon chemical fiber.
Detailed Description
Example 1
Dispersing 2000kg of pigment-grade anatase titanium dioxide in 2000kg of deionized water, adding 6kg of sodium polyacrylate dispersant, and dispersing for 45 minutes by using a high-speed dispersion machine to prepare slurry; grinding the slurry twice by a grinder, transferring the slurry into a stirring kettle, adding 8000kg of deionized water into the slurry for dilution, continuously feeding the diluted slurry into a horizontal spiral discharging centrifugal classifier for classification, removing large-particle materials, and feeding fine-particle materials into the stirring kettle. Heating the slurry to 80 ℃, adding 8kg of antimony trichloride into the slurry under continuous stirring, continuously stirring for 30 minutes, slowly adding 40kg of 10% sodium hydroxide into the slurry, and controlling the adding time to be 3 hours; adding 120kg of zirconium oxychloride octahydrate into the slurry under continuous stirring, continuously stirring for 30 minutes, slowly adding 300kg of 10% sodium hydroxide into the slurry, and controlling the adding time to be 3 hours; stirring is continued for 30 minutes, the slurry is sent into a plate-and-frame filter press for filtration, and the filter cake is washed by deionized water until no chloride ion exists.
Putting the filter cake into a pulping tank, adding 3000kg of deionized water into the filter cake for pulping, adding 7kg of sodium polyacrylate dispersant into the slurry, stirring for 30 minutes, weighing 5kg of pentaerythritol, adding the pentaerythritol into the slurry, and stirring for 1 hour to obtain the TiO with the pentaerythritol modified surface and uniform dispersion2And (3) sizing agent, drying the sizing agent, crushing the dried material by using a crusher, and packaging to obtain the titanium dioxide for the nylon chemical fiber.
Example 2
Dispersing 2000kg of pigment-grade anatase titanium dioxide in 2000kg of deionized water, adding 7kg of sodium polyacrylate dispersant, and dispersing for 50 minutes by using a high-speed dispersion machine to prepare slurry; grinding the slurry twice by a grinder, transferring the slurry into a stirring kettle, adding 8000kg of deionized water into the slurry for dilution, continuously feeding the diluted slurry into a horizontal spiral discharging centrifugal classifier for classification, removing large-particle materials, and feeding fine-particle materials into the stirring kettle. Heating the slurry to 80 ℃, adding 12kg of antimony trichloride into the slurry under continuous stirring, continuously stirring for 30 minutes, slowly adding 60kg of 10% sodium hydroxide into the slurry, and controlling the adding time to be 3 hours; adding 150kg of zirconium oxychloride octahydrate into the slurry under continuous stirring, continuously stirring for 30 minutes, slowly adding 400kg of 10% sodium hydroxide into the slurry, and controlling the adding time to be 3 hours; stirring is continued for 30 minutes, the slurry is sent into a plate-and-frame filter press for filtration, and the filter cake is washed by deionized water until no chloride ion exists.
Putting the filter cake into a pulping tank, adding 3000kg of deionized water into the filter cake for pulping, adding 8kg of sodium polyacrylate dispersant into the slurry, stirring for 30 minutes, weighing 10kg of pentaerythritol, adding into the slurry, and stirring for 1 hour to obtain the TiO with the pentaerythritol modified surface and uniform dispersion2And (3) sizing agent, drying the sizing agent, crushing the dried material by using a crusher, and packaging to obtain the titanium dioxide for the nylon chemical fiber.
Example 3
Dispersing 2000kg of pigment-grade anatase titanium dioxide in 2000kg of deionized water, adding 4kg of sodium polyacrylate dispersant, and dispersing for 30 minutes by using a high-speed dispersion machine to prepare slurry; grinding the slurry twice by a grinder, transferring the slurry into a stirring kettle, adding 8000kg of deionized water into the slurry for dilution, continuously feeding the diluted slurry into a horizontal spiral discharging centrifugal classifier for classification, removing large-particle materials, and feeding fine-particle materials into the stirring kettle. Heating the slurry to 80 ℃, adding 10kg of antimony trichloride into the slurry under continuous stirring, continuously stirring for 30 minutes, slowly adding 50kg of 10% sodium hydroxide into the slurry, and controlling the adding time to be 3 hours; adding 130kg of zirconium oxychloride octahydrate into the slurry under continuous stirring, continuously stirring for 30 minutes, slowly adding 350kg of 10% sodium hydroxide into the slurry, and controlling the adding time to be 3 hours; stirring is continued for 30 minutes, the slurry is sent into a plate-and-frame filter press for filtration, and the filter cake is washed by deionized water until no chloride ion exists.
Putting the filter cake into a pulping tank, adding 3000kg of deionized water into the filter cake for pulping, adding 6kg of sodium polyacrylate dispersant into the slurry, stirring for 30 minutes, weighing 8kg of pentaerythritol, adding into the slurry, and stirring for 1 hour to obtain the TiO with the surface modified by the pentaerythritol and uniformly dispersed2And (3) sizing agent, drying the sizing agent, crushing the dried material by using a crusher, and packaging to obtain the titanium dioxide for the nylon chemical fiber.
Example 4
Dispersing 2000kg of pigment-grade anatase titanium dioxide in 2000kg of deionized water, adding 5kg of sodium polyacrylate dispersant, and dispersing for 40 minutes by using a high-speed dispersion machine to prepare slurry; grinding the slurry twice by a grinder, transferring the slurry into a stirring kettle, adding 8000kg of deionized water into the slurry for dilution, continuously feeding the diluted slurry into a horizontal spiral discharging centrifugal classifier for classification, removing large-particle materials, and feeding fine-particle materials into the stirring kettle. Heating the slurry to 80 ℃, adding 11kg of antimony trichloride into the slurry under continuous stirring, continuously stirring for 30 minutes, slowly adding 48kg of 10% sodium hydroxide into the slurry, and controlling the adding time to be 3 hours; adding 130kg of zirconium oxychloride octahydrate into the slurry under continuous stirring, continuously stirring for 30 minutes, slowly adding 380kg of 10% sodium hydroxide into the slurry, and controlling the adding time to be 3 hours; stirring is continued for 30 minutes, the slurry is sent into a plate-and-frame filter press for filtration, and the filter cake is washed by deionized water until no chloride ion exists.
Putting the filter cake into a pulping tank, adding 3000kg of deionized water into the filter cake for pulping, adding 6.8kg of sodium polyacrylate dispersant into the slurry, stirring for 30 minutes, weighing 6kg of pentaerythritol, adding into the slurry, stirring for 1 hour to obtain the TiO with the surface modified by the pentaerythritol and uniformly dispersed2And (3) sizing agent, drying the sizing agent, crushing the dried material by using a crusher, and packaging to obtain the titanium dioxide for the nylon chemical fiber.
Example 5
Dispersing 2000kg of pigment-grade anatase titanium dioxide in 2000kg of deionized water, adding 4kg of sodium polyacrylate dispersant, and dispersing for 60 minutes by using a high-speed dispersion machine to prepare slurry; grinding the slurry twice by a grinder, transferring the slurry into a stirring kettle, adding 8000kg of deionized water into the slurry for dilution, continuously feeding the diluted slurry into a horizontal spiral discharging centrifugal classifier for classification, removing large-particle materials, and feeding fine-particle materials into the stirring kettle. Heating the slurry to 80 ℃, adding 9kg of antimony trichloride into the slurry under continuous stirring, continuously stirring for 30 minutes, slowly adding 42kg of 10% sodium hydroxide into the slurry, and controlling the adding time to be 3 hours; adding 140kg of zirconium oxychloride octahydrate into the slurry under continuous stirring, continuously stirring for 30 minutes, slowly adding 390kg of 10% sodium hydroxide into the slurry, and controlling the adding time to be 3 hours; stirring is continued for 30 minutes, the slurry is sent into a plate-and-frame filter press for filtration, and the filter cake is washed by deionized water until no chloride ion exists.
Putting the filter cake into a pulping tank, adding 3000kg of deionized water into the filter cake for pulping, adding 7.4kg of sodium polyacrylate dispersant into the slurry, stirring for 30 minutes, weighing 9kg of pentaerythritol, adding the pentaerythritol into the slurry, and stirring for 1 hour to obtain the TiO with the pentaerythritol modified surface and uniform dispersion2And (3) sizing agent, drying the sizing agent, crushing the dried material by using a crusher, and packaging to obtain the titanium dioxide for the nylon chemical fiber.
Example 6
Dispersing 2000kg of pigment-grade anatase titanium dioxide in 2000kg of deionized water, adding 4kg of sodium polyacrylate dispersant, and dispersing for 30 minutes by using a high-speed dispersion machine to prepare slurry; grinding the slurry twice by a grinder, transferring the slurry into a stirring kettle, adding 8000kg of deionized water into the slurry for dilution, continuously feeding the diluted slurry into a horizontal spiral discharging centrifugal classifier for classification, removing large-particle materials, and feeding fine-particle materials into the stirring kettle. Heating the slurry to 80 ℃, adding 8.8kg of antimony trichloride into the slurry under continuous stirring, continuously stirring for 30 minutes, slowly adding 43kg of 10% sodium hydroxide into the slurry, and controlling the adding time to be 3 hours; adding 128kg of zirconium oxychloride octahydrate into the slurry under continuous stirring, continuously stirring for 30 minutes, slowly adding 330kg of 10% sodium hydroxide into the slurry, and controlling the adding time to be 3 hours; stirring is continued for 30 minutes, the slurry is sent into a plate-and-frame filter press for filtration, and the filter cake is washed by deionized water until no chloride ion exists.
Putting the filter cake into a pulping tank, adding 3000kg of deionized water into the filter cake for pulping, adding 7.8kg of sodium polyacrylate dispersant into the slurry, stirring for 30 minutes, weighing 7.5kg of pentaerythritol, adding the pentaerythritol into the slurry, and stirring for 1 hour to obtain the TiO with the pentaerythritol modified surface and uniform dispersion2Drying the slurry, pulverizing the dried material with a pulverizer, and packaging to obtain chinlonTitanium dioxide for fibers.
Example 7
In the prior art, hydrated silicon oxide and hydrated alumina are adopted to coat titanium dioxide for delustring of polyamide chemical fiber: the fouling period of the heat exchanger tube array of the prepolymerization tower is less than 3 months, and the fouling period of the tube array of the triple-effect evaporator is less than 3 months;
example 1 titanium dioxide for delustering polyamide chemical fiber: the fouling period of the heat exchanger tube array of the prepolymerization tower is more than 12 months, and the fouling period of the tube array of the triple-effect evaporator is more than 12 months;
example 2 titanium dioxide for delustering polyamide chemical fiber: the fouling period of the heat exchanger tube array of the prepolymerization tower is more than 12 months, and the fouling period of the tube array of the triple-effect evaporator is more than 12 months;
example 3 titanium dioxide for delustering chinlon chemical fiber: the fouling period of the heat exchanger tube array of the prepolymerization tower is more than 12 months, and the fouling period of the tube array of the triple-effect evaporator is more than 12 months;
example 4 titanium dioxide for delustering chinlon chemical fiber: the fouling period of the heat exchanger tube array of the prepolymerization tower is more than 12 months, and the fouling period of the tube array of the triple-effect evaporator is more than 12 months;
example 5 titanium dioxide for delustering chinlon chemical fiber: the fouling period of the heat exchanger tube array of the prepolymerization tower is more than 12 months, and the fouling period of the tube array of the triple-effect evaporator is more than 12 months;
example 6 titanium dioxide for delustering nylon chemical fibers: the fouling period of the heat exchanger tube array of the prepolymerization tower is more than 12 months, and the fouling period of the tube array of the triple-effect evaporator is more than 12 months.
Claims (4)
1. A preparation method of titanium dioxide for delustering chinlon chemical fibers is characterized by comprising the following steps: dispersing pigment-grade anatase titanium dioxide into water slurry, and grinding, diluting and grading to remove large particles; then coating antimony oxide and hydrated zirconium oxide on the surfaces of the titanium dioxide particles; and then pentaerythritol is used for treating the surface of the inorganic coated titanium dioxide particles to obtain the titanium dioxide for delustering the nylon chemical fiber.
2. The method of claim 1, wherein the pigment-grade anatase titanium dioxide is dispersed in an aqueous slurry and ground, diluted, and classified to remove large particles, wherein the method comprises the steps of: dispersing 200 parts by weight of pigment-grade anatase titanium dioxide in 200 parts by weight of deionized water, adding 0.4-0.8 part by weight of sodium polyacrylate dispersant, and dispersing for 30-60 minutes by using a high-speed dispersion machine to prepare slurry; grinding the slurry twice by using a grinder, then transferring the slurry into a stirring kettle, adding 800 parts of deionized water into the slurry for dilution, continuously feeding the diluted slurry into a horizontal spiral discharging centrifugal classifier for classification, removing large-particle materials, and feeding fine-particle materials into the stirring kettle for later use.
3. The method of claim 1, wherein the surface of the titanium dioxide particles is coated with antimony oxide, hydrous zirconium oxide, and wherein: heating the slurry to 80 ℃, adding 0.8-1.2 parts of antimony trichloride into the slurry under continuous stirring, continuously stirring for 30 minutes, slowly adding 4-6 parts of 10% sodium hydroxide into the slurry, and controlling the adding time to be 3 hours; adding 12-15 parts of zirconium oxychloride octahydrate into the slurry under continuous stirring, continuously stirring for 30 minutes, slowly adding 30-40 parts of 10% sodium hydroxide into the slurry, and controlling the adding time to be 3 hours; stirring is continued for 30 minutes, the slurry is sent into a plate-and-frame filter press for filtration, and the filter cake is washed by deionized water until no chloride ion exists.
4. The method of claim 1, wherein the surface of the inorganic coated titanium dioxide particles is treated with pentaerythritol, characterized in that: putting the filter cake into a pulping tank, adding 300 parts of deionized water into the filter cake for pulping, adding 0.6-0.8 part of sodium polyacrylate dispersant into the pulp, stirring for 30 minutes, weighing 0.5-1.0 part of pentaerythritol, adding the pentaerythritol into the pulp, and stirring for 1 hour to obtain the TiO with the surface modified by the pentaerythritol and uniformly dispersed2And (3) sizing agent, drying the sizing agent, crushing the dried material by using a crusher, and packaging to obtain the titanium dioxide for the nylon chemical fiber.
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