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Preparation method of full-wavelength ultraviolet shielding pearlescent pigment

A pearlescent pigment and external shielding technology, which is applied in the field of pearlescent pigments, can solve the problems such as difficult to accurately control the dropping rate of alkaline substances and reduce the pH value of the reaction system, so as to facilitate promotion and use, good product performance, and strong ultraviolet shielding ability Effect

Pending Publication Date: 2022-05-06
ZHEJIANG COLORAY TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The existing pearlescent pigment production process is mainly the liquid phase deposition method, that is, in the aqueous solution state, the hydrolysis reaction of the metal salt is used to generate the corresponding metal oxide or hydroxide, and the hydrolyzed product is separated by Coulomb force and van der Waals force. Adsorbed on the surface of the substrate, the metal salts in it are mainly chloride salts, and the main by-product generated after hydrolysis of chloride salts is HCl, which will reduce the pH value of the reaction system and affect the progress of the reaction. Therefore, in the prior art The excess H is usually neutralized by adding an additional alkaline substance + , to achieve the effect of stabilizing the pH, but it is difficult to accurately control the dropping rate of the alkaline substance in the actual operation process, and it cannot affect the Cl in the reaction solution. - For removal, a large amount of Cl will be produced - waste water

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Preparation of reaction aid particles

[0029] S1: Weigh 243.1g of magnesium nitrate hexahydrate and 375.79g of aluminum nitrate nonahydrate and stir and dissolve them in 2L of water to obtain a mixed salt solution. Add 30.06g of nanometer ferric oxide to the mixed salt solution at a speed of 800-1000r / min Stir and disperse, then add 206.42g of tetrapropylammonium hydroxide, then add 684.96g of urea, dissolve the urea in 1.2L of water before adding, heat up to 50°C, keep stirring for 20-30min, then place at 150-160°C temperature, heat preservation and crystallization for 24 hours, take out and cool to room temperature for filtration, wash the filter cake with deionized water and centrifuge until the pH value of the supernatant is 7-8, and dry for 6-12 hours to obtain the hydrotalcite precursor;

[0030] S2: Take 200g of hydrotalcite precursor, under nitrogen atmosphere, at 2°C·min -1 The heating rate is increased to 500 ° C, roasted for 5 hours, and cooled to room temp...

Embodiment 2

[0036] 反应助剂颗粒的制备

[0037] S1:称取534.83g六水合硝酸镁、750.26g九水合硝酸铝搅拌溶解于2L水中,得到混合盐溶液,向混合盐溶液中加入45.06g纳米四氧化三铁,以800-1000r / min的速度进行搅拌分散,然后加入382.17g四丙基氢氧化铵,再加入1546.34g尿素,尿素溶解于3L水中后加入,升温至50℃,保温搅拌20-30min,再置于150-160℃温度下,保温晶化24h后,取出冷却至室温过滤,滤饼用去离子水洗涤离心至上清液pH值为7-8,干燥6-12h,得水滑石前体;

[0038] S2:取150g水滑石前体,在氮气气氛下,以10℃·min -1 的升温速率升温至400℃,焙烧12h,冷却至室温,得到复合氧化物;

[0039] S3:称取NaOH溶于去离子水中得到浓度为1mol / L氢氧化钠溶液,称取15g复合氧化物,置于1200mL氢氧化钠溶液中,磁力搅拌2-12h,过滤,滤饼用去离子水洗涤离心至上清液pH值为7-8,干燥12-15h,得到反应助剂颗粒。

[0040] 全波长紫外屏蔽珠光颜料的制备

[0041] 基材预处理:称取0.85g过氧化苯甲酰搅拌溶解于30mL二甲基亚砜中,得到过氧化苯甲酰溶液,称取10g超细片状云母超声分散于100mL二甲基亚砜中,加入4g N-(3-磺丙基)-N-(丙烯酰氧乙基)-N,N-二甲基碱搅拌溶解后,滴加加入过氧化苯甲酰溶液,搅拌混匀后,油浴升温至90℃,搅拌保温反应40h,降至室温,过滤,滤饼先用无水乙醇洗涤2次,再用90℃去离子洗涤3次,于110℃温度下真空干燥。

[0042] 称取氢氧化钠搅拌溶解于水中,配制得到浓度为1.5mol / L氢氧化钠水溶液,量取53.0mL氢氧化钠水溶液,加入5g经过预处理的基材,加入1.2g反应助剂颗粒,搅拌分散后,水浴加热至50℃,得到反应基液,将20.0mL、2.0mol / L TiCl 4 水溶液以3.0mL / min的速度滴加到反应基液中,滴加完成后,升温至80℃,保温晶化2h,然后加入20ml 1.0mol / L ZnCl 2 溶液,再加入1.0mol / L Na 2 CO 3 溶液中和体系至中性,反应完成,通过磁分离去除反应助剂颗粒,抽滤,用去离子水洗涤至滤液无Cl - (1.0mol / L Ag...

Embodiment 3

[0044] 反应助剂颗粒的制备

[0045] S1:称取769.20g六水合硝酸镁、1125.39g九水合硝酸铝搅拌溶解于2L水中,得到混合盐溶液,向混合盐溶液中加入78.78g纳米四氧化三铁,以800-1000r / min的速度进行搅拌分散,然后加入712.48g四丙基氢氧化铵,再加入3245.86g尿素,尿素溶解于10L水中后加入,升温至50℃,保温搅拌20-30min,再置于150-160℃温度下,保温晶化24h后,取出冷却至室温过滤,滤饼用去离子水洗涤离心至上清液pH值为7-8,干燥6-12h,得水滑石前体,;

[0046] S2:取100g水滑石前体,在氮气气氛下,以8℃·min -1 的升温速率升温至600℃,焙烧2h,冷却至室温,得到复合氧化物;

[0047] S3:称取NaOH溶于去离子水中得到浓度为1mol / L氢氧化钠溶液,称取2g复合氧化物,置于500mL氢氧化钠溶液中,磁力搅拌2-12h,过滤,滤饼用去离子水洗涤离心至上清液pH值为7-8,干燥12-15h,得到反应助剂颗粒。

[0048] 全波长紫外屏蔽珠光颜料的制备

[0049] 基材预处理:称取0.85g过氧化苯甲酰搅拌溶解于30mL二甲基亚砜中,得到过氧化苯甲酰溶液,称取11g片状玻璃鳞片超声分散于100mL二甲基亚砜中,加入5g N-(3-磺丙基)-N-(丙烯酰氧乙基)-N,N-二甲基碱搅拌溶解后,滴加加入过氧化苯甲酰溶液,搅拌混匀后,油浴升温至95℃,搅拌保温反应24h,降至室温,过滤,滤饼先用无水乙醇洗涤2-3次,再用90℃去离子洗涤2-3次,于100℃温度下真空干燥

[0050] 称取氢氧化钠搅拌溶解于水中,配制得到浓度为1.5mol / L氢氧化钠水溶液,量取53.0mL氢氧化钠水溶液,加入5g经过预处理的基材,加入1.5g反应助剂颗粒,搅拌分散后,水浴加热至50℃,得到反应基液,将20.0mL、2.0mol / L TiCl 4 水溶液以4.0mL / min的速度滴加到反应基液中,滴加完成后,升温至80℃,保温晶化2h,然后加入120ml 1.0mol / L ZnCl 2 溶液,再加入1.0mol / L Na 2 CO 3 溶液中和体系至中性,反应完成,通过磁分离去除反应助剂颗粒,抽滤,用去离子水洗涤至滤液无Cl - (1.0mol...

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Abstract

The invention discloses a preparation method of a full-wavelength ultraviolet shielding pearlescent pigment, and relates to the technical field of pearlescent pigments. The preparation method specifically comprises the following steps: S1, stirring and dissolving sodium hydroxide in water to obtain a sodium hydroxide solution and a pretreated base material, then adding reaction aid particles, stirring and dispersing, and heating to 50-65 DEG C to obtain a reaction base solution; s2, dropwise adding a TiCl4 aqueous solution into the reaction base solution, heating to 80 DEG C after dropwise adding, and carrying out heat preservation crystallization for 2 hours; and S3, then adding a ZnCl2 solution, then adding a Na2CO3 solution to adjust the pH value to be neutral, carrying out suction filtration after the reaction is completed, washing a filter cake with deionized water until no Cl <-> exists in the filtrate, drying and crushing the filter cake, removing reaction auxiliary agent particles, and calcining. The invention discloses a preparation method of a full-wavelength ultraviolet shielding pearlescent pigment, which is characterized in that reaction aid particles are added into a reaction solution, so that the pH value of the reaction solution can be adjusted, Cl <-> in the reaction solution can be removed, and the problem that a large amount of chlorine-containing wastewater is generated is avoided.

Description

technical field [0001] The invention relates to the technical field of pearlescent pigments, in particular to a preparation method of full-wavelength ultraviolet shielding pearlescent pigments. Background technique [0002] In recent years, with the gradual destruction of the ozone layer and the increase of ultraviolet radiation, the intensity of ultraviolet rays on the ground has continued to increase. Excessive exposure to ultraviolet rays will lead to redness, swelling, peeling and aging of the human body. In severe cases, it will cause skin cancer. Ultraviolet rays have strong penetrating ability , can cause skin tanning, aging and DNA damage, so research on anti-ultraviolet products has gradually become a hot field. [0003] Pearlescent pigments are named for their soft luster like pearls. The main preparation method is to uniformly coat a single layer or multiple layers of metal oxide on the surface of the substrate, so that the light can undergo multiple reflections a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09C1/00C09C1/40C09C1/30C09C3/06
CPCC09C1/0015C09C1/0024C09C3/063C09C3/006C09C2200/102
Inventor 卓仲标唐骏
Owner ZHEJIANG COLORAY TECH DEV