CN104071842B - The preparation method of pearl white - Google Patents
The preparation method of pearl white Download PDFInfo
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- CN104071842B CN104071842B CN201310106791.1A CN201310106791A CN104071842B CN 104071842 B CN104071842 B CN 104071842B CN 201310106791 A CN201310106791 A CN 201310106791A CN 104071842 B CN104071842 B CN 104071842B
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Abstract
The invention provides a kind of preparation method of pearl white, comprise the following steps: under the effect of nonionogenic tenside, bismuth mixed salt solution reacts under constant pH condition, obtains bismuth oxychloride crystals; Described bismuth mixed salt solution comprises bismuth ion, chlorion, nitrate ion and water.Preparation method provided by the invention, by regulating constant pH and selecting suitable nonionogenic tenside, makes the formation speed, shape, size etc. of pearl white all controlled, thus prepare the bismuth oxychloride crystals of micron level, and its size is controlled.
Description
Technical field
The invention belongs to Inorganic synthese technical field, particularly relate to a kind of preparation method of pearl white.
Background technology
Pearly pigment can show the effect of pearlescent by the reflection of light, because it is specious, be widely used in all kinds of material.The main raw material of pearly pigment is natural pearl powder, and it extracts by fish scale and air bladder, but expensive, therefore needs low-cost substitute.Pearl white and white lead carbonate are tabular crystal structure, have higher specific refractory power, high gloss, can show the effect of similar pearlescent, be thus often used as the substitute of natural peral powder by the reflection of light.But comprise highly toxic substance lead in white lead carbonate, Long Term Contact can impact the healthy of people, therefore along with the requirement of environment protection, white lead carbonate is used by the restriction of increasing countries and regions; And pearl white has nontoxic, environmental protection, Low grease absorbs, skin adhesion is strong and the feature such as good pearl effect, be considered to the good substitute of natural peral powder.
Pearl white has another name called Bismuth Oxychloride, and molecular formula is BiOCl, and pearl white is alkaline bismuth salt, and the shinny crystalline powder of tetragonal spheroidal silvery white flake, has kneaded open silvery white pearliness; Be dissolved in hydrochloric acid and nitric acid, water insoluble, acetone, tartrate and ammonia.
Prior art discloses the synthetic method of multiple pearl white, as simple radical health etc. discloses a kind of method utilizing solvent-thermal method to prepare BiOCl single-chip, the steps include: first by BiCl
3and KBH
4put into deionized water and dehydrated alcohol mixing solutions in proportion, carry out stirring reaction, and then mixing solutions is put into teflon-lined stainless steel autoclave, carry out solvent thermal reaction at high temperature under high pressure 16 ~ 24 hours, finally carry out aftertreatment and obtain BiOCl single-chip.
Li Yadongs etc. disclose the synthetic method utilizing hydrothermal method to prepare bismuth oxychloride pearlescent pigment, the steps include: first by Bi (NO
3)
35H
2o and cetyl chloride ammonium put into deionized water in proportion, carry out stirring reaction, then NaOH solution is put into wherein, carry out stirring reaction, again mixing solutions is put into teflon-lined stainless steel autoclave, and reactor is put into baking oven and carry out hydro-thermal reaction 8 ~ 24 hours, finally carry out aftertreatment and obtain bismuth oxychloride pearlescent pigment.
But the pearl white size of above-mentioned solvent-thermal method and water heat transfer is little and uncontrollable, is generally Nano grade, be difficult to the requirement meeting different application field.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is the preparation method providing a kind of pearl white, and method provided by the invention can prepare the pearl white of micron level, and size is controlled.
The invention discloses a kind of preparation method of pearl white, comprise the following steps:
A) under the effect of nonionogenic tenside, bismuth mixed salt solution reacts under constant pH condition, obtains pearl white; Described bismuth mixed salt solution comprises bismuth ion, chlorion, nitrate ion and water.
Preferably, described constant pH is 0.1 ~ 4.0.
Preferably, described nonionogenic tenside be in OP emulsifying agent, tween emulsifier type, oleyl amine, fatty alcohol-polyoxyethylene ether, spans emulsifying agent, polyoxyethylene glycol, oleic acid and polyvinyl alcohol one or more.
Preferably, the temperature of described reaction is 60 ~ 85 DEG C, and the time of described reaction is 10 ~ 20 hours.
Preferably, described steps A) be specially:
A1) hydrochloric acid and deionized water are mixed, obtain mixing solutions;
A2) in described mixing solutions, add nonionogenic tenside, then add bismuth mixed salt solution and react, add NaOH solution while adding bismuth mixed salt solution and keep reaction mixture pH value constant, after reaction, obtain bismuth oxychloride crystals.
Preferably, described steps A 2) also comprise before:
By described steps A 1) mixing solutions that obtains is heated to 60 ~ 85 DEG C.
Preferably, the quality of described nonionogenic tenside and the volume ratio of deionized water are (0.5 ~ 1.5g): 1L.
Preferably, in described bismuth mixed salt solution, the concentration of bismuth ion is 1.5 ~ 2.5mol/L.
Preferably, described bismuth mixed salt solution be that Bismuth trinitrate is dissolved in hydrochloric acid, bismuth chloride is dissolved in nitric acid and bismuth oxide is dissolved in the mixed solution of nitric acid and hydrochloric acid one or more.
Preferably, described steps A 2) be specially:
A21) in described mixing solutions, add nonionogenic tenside, then drip bismuth mixed salt solution and react, drip NaOH solution while adding bismuth mixed salt solution and keep reaction mixture pH value constant;
A22) after bismuth mixed salt solution dropwises, continue to add NaOH solution to reaction mixture, until reaction mixture pH value is 8.0 ~ 11.0 rear stopped reaction, obtain bismuth oxychloride crystals.
The invention provides a kind of preparation method of bismuth oxychloride crystals, under the effect of nonionogenic tenside, to comprise the bismuth mixed salt solution of bismuth ion, chlorion, nitrate ion and water for raw material, react under constant pH value condition, can bismuth oxychloride crystals be obtained.Compared with prior art, the bismuth mixed salt solution that the present invention makes to comprise bismuth ion, chlorion, nitrate ion and water reacts under the effect of nonionogenic tenside and constant pH, by regulating constant pH and selecting suitable nonionogenic tenside, make the formation speed, shape, size etc. of pearl white all controlled, thus prepare the pearl white of micron level, and its size is controlled.Experimental result shows, the pearl white that the present invention prepares is thin plate crystal, and particle diameter is micron level.
Accompanying drawing explanation
Fig. 1 is the pearl white scanning electron microscope diagram of preparation in the embodiment of the present invention 1;
Fig. 2 is the XRD diffracting spectrum of the pearl white of preparation in the embodiment of the present invention 1;
Fig. 3 is the pearl white scanning electron microscope diagram of preparation in the embodiment of the present invention 2;
Fig. 4 is the pearl white scanning electron microscope diagram of preparation in the embodiment of the present invention 3;
Fig. 5 is the pearl white scanning electron microscope diagram of preparation in the embodiment of the present invention 4;
Fig. 6 is the pearl white scanning electron microscope diagram of preparation in the embodiment of the present invention 5;
Fig. 7 is the pearl white scanning electron microscope diagram of preparation in the embodiment of the present invention 6;
Fig. 8 is the pearl white scanning electron microscope diagram of preparation in the embodiment of the present invention 7.
Embodiment
In order to understand the present invention further, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these describe just in order to further illustrate the features and advantages of the present invention, instead of the restriction to invention claim.
The invention provides a kind of preparation method of bismuth oxychloride crystals, comprise the following steps:
Under the effect of nonionogenic tenside, bismuth mixed salt solution reacts under constant pH condition, obtains bismuth oxychloride crystals; Described bismuth mixed salt solution comprises bismuth ion, chlorion, nitrate ion and water.
The present invention is under the effect of nonionogenic tenside, the bismuth mixed salt solution comprising bismuth ion, chlorion, nitrate ion and water is reacted under the effect of constant pH, by regulating constant pH and selecting suitable nonionogenic tenside, make the formation speed, shape, size etc. of bismuth oxychloride crystals all controlled, thus prepare the pearl white of micron level, and its size is controlled.
The all raw materials of the present invention, are not particularly limited its source, commercially buy.
The present invention is with bismuth mixed salt solution for reaction raw materials, and described bismuth mixed salt solution comprises bismuth ion, chlorion, nitrate ion and water; Described bismuth mixed salt solution is preferably that Bismuth trinitrate is dissolved in hydrochloric acid, bismuth chloride is dissolved in nitric acid and bismuth oxide is dissolved in the mixed solution of nitric acid and hydrochloric acid one or more, be more preferably Bismuth trinitrate and be dissolved in hydrochloric acid; In described bismuth mixed salt solution, bismuth concentration is preferably 1.5 ~ 2.5mol/L, is more preferably 1.8 ~ 2.3mol/L; The present invention is not particularly limited the concentration of chlorion, nitrate ion in described bismuth mixed salt solution, can meet the concentration requirement of bismuth ion; The raw material sources of the present invention to described bismuth mixed salt solution are not particularly limited, and obtain with ordinary method well known to those skilled in the art.
Bismuth mixed salt solution of the present invention reacts under the effect of nonionogenic tenside, described nonionogenic tenside to be preferably in OP emulsifying agent, tween emulsifier type, oleyl amine, fatty alcohol-polyoxyethylene ether, spans emulsifying agent, polyoxyethylene glycol, oleic acid and polyvinyl alcohol one or more, is more preferably one or more in OP emulsifying agent, Tweens and oleyl amine; In the quality of described nonionogenic tenside and bismuth mixed salt solution, the mole number ratio of bismuth ion is preferably 1g:(0.019 ~ 0.072mol), be more preferably 1g:(0.03 ~ 0.06mol).
The present invention, under the effect of nonionogenic tenside, makes the bismuth mixed salt solution comprising bismuth ion, chlorion, nitrate ion and water react under constant pH condition, obtains pearl white, and this process is preferably:
A1) hydrochloric acid and deionized water are mixed, obtain mixing solutions;
A2) in described mixing solutions, add nonionogenic tenside, then add bismuth mixed salt solution and react, add NaOH solution while adding bismuth mixed salt solution and keep reaction mixture pH value constant, after reaction, obtain pearl white.
Hydrochloric acid and deionized water first first mix by the present invention, obtain mixing solutions, and the pH value of described mixing solutions is preferably 0.1 ~ 4, is more preferably 0.5 ~ 3.0.
After obtaining mixing solutions, add nonionogenic tenside wherein, in the quality of described nonionogenic tenside and described mixing solutions, the volume ratio of deionized water is preferably (0.5 ~ 1.5g): 1L, is more preferably (0.7 ~ 1.3g): 1L.
Described mixing solutions, before adding nonionogenic tenside, preferably stirs and heats, being preferably heated to 60 ~ 85 DEG C, being more preferably heated to 65 ~ 75 DEG C by the present invention.The present invention is not particularly limited the mode stirred and heat, mode well known to those skilled in the art.
After adding nonionogenic tenside, add bismuth mixed salt solution wherein, add sodium hydroxide solution keeps reacting liquid pH value constant simultaneously, and bismuth mixed salt solution reacts under the condition of nonionogenic tenside, constant pH and heating, obtains bismuth oxychloride crystals.
Reaction formula is as follows:
Bi(NO
3)
3+HCl+H
2O→BiOCl+3HNO
3
In the present invention, described constant pH is preferably 0.1 ~ 4.0, is more preferably 0.5 ~ 3.0; The temperature of described reaction is preferably 60 ~ 85 DEG C, is more preferably 65 ~ 75 DEG C; The time of described reaction is preferably 10 ~ 20 hours, is more preferably 12 ~ 17 hours.
Specifically, the present invention preferably operates according to following steps:
A21) in described mixing solutions, add nonionogenic tenside, then drip bismuth mixed salt solution and react, drip NaOH solution while adding bismuth mixed salt solution and keep reaction mixture pH value constant;
A22) after bismuth mixed salt solution dropwises, continue to add NaOH solution to reaction mixture, until reaction mixture pH value is 8.0 ~ 11.0 rear stopped reaction, obtain bismuth oxychloride crystals.
After adding nonionogenic tenside, the present invention preferably drips bismuth mixed salt solution and reacts, and drips sodium hydroxide solution simultaneously and keeps reaction mixture pH value constant.The time for adding of described bismuth mixed salt solution is preferably 10 ~ 20 hours, is more preferably 12 ~ 17 hours; The rate of addition of described bismuth mixed salt solution is preferably 0.02 ~ 0.06ml/min, is more preferably 0.03 ~ 0.05ml/min.
The present invention, after bismuth mixed salt solution dropwises, continues to drip sodium hydroxide solution, and be 8.0 ~ 11.0 rear stopped reaction to reaction mixture pH value, can obtain bismuth oxychloride crystals, detailed process is preferably carried out according to following steps:
After reaction terminates, continue to drip NaOH solution in reaction mixture, heat until reaction mixture pH value is 8.0 ~ 11.0 rear stoppings and stirs, reaction mixture is down to room temperature, obtains solid product bismuth oxychloride crystals through washing, filtration aftertreatment.Described reaction mixture pH value is preferably 8.0 ~ 11.0, is more preferably 9.0 ~ 10.0; Described washing is preferably washed with distilled water.The mode of the present invention to washing and filtration is not particularly limited, with usual manner well known to those skilled in the art.
Carry out sem observation to pearl white, result shows, products therefrom presents tetragon, octagon or irregular thin plate crystal, and particle diameter is micron level.
In order to understand the present invention further, below in conjunction with embodiment, the preparation method to pearl white provided by the invention is described in detail, and protection scope of the present invention is not limited by the following examples.
Embodiment 1
Bismuth chloride is dissolved in nitric acid, prepares the bismuth mixed salt solution that bismuth concentration is 2.0mol/L.
In the reaction vessel of 5L, add 1.5L deionized water, open and stir and add hydrochloric acid, adjust ph is 0.1, and above-mentioned mixing solutions is heated to 75 DEG C, adds the OP emulsifying agent that 1g molecular weight is 646, under the condition of constant temperature, to the above-mentioned bismuth mixed salt solution of the mixed solution and dripping adding OP emulsifying agent, rate of addition is 0.06ml/min, and slowly adds 6mol/LNaOH solution simultaneously and keep pH value to be 0.1.After 10 hours, stop adding bismuth mixed salt solution, continue to add NaOH solution, until reaction mixture pH value is 8.0, stops heating and stir, being down to room temperature, after filtering with distilled water wash, obtaining pearl white.
Carry out sem observation to pearl white, result is the pearl white scanning electron microscope diagram of preparation in the embodiment of the present invention 1 see Fig. 1, Fig. 1, and as shown in Figure 1, products therefrom presents irregular thin plate crystal, and particle diameter is 2 ~ 5 microns.
Carry out XRD diffraction to described pearl white, result is the XRD diffracting spectrum of the pearl white of preparation in the embodiment of the present invention 1 see Fig. 2, Fig. 2, and as shown in Figure 2, product prepared by the present invention is bismuth oxychloride crystals.
Embodiment 2
Bismuth chloride is dissolved in nitric acid, prepares the bismuth mixed salt solution that bismuth concentration is 2.2mol/L.
In the reaction vessel of 5L, add 1.5L deionized water, open and stir and add hydrochloric acid, adjust ph is 2.0, and above-mentioned mixing solutions is heated to 85 DEG C, adds 0.5g tween 80, under the condition of constant temperature, to the above-mentioned bismuth mixed salt solution of the mixed solution and dripping adding tween 80, rate of addition is 0.03ml/min, and slowly adds 6mol/LNaOH solution simultaneously and keep pH value to be 2.0.After 11 hours, stop adding bismuth mixed salt solution, continue to add NaOH solution, until reaction mixture pH value is 9.0, stops heating and stir, being down to room temperature, after filtering with distilled water wash, obtaining bismuth oxychloride crystals.
Carry out sem observation to pearl white, result is the pearl white scanning electron microscope diagram of preparation in the embodiment of the present invention 2 see Fig. 3, Fig. 3, and as shown in Figure 3, products therefrom presents irregular thin plate crystal, and particle diameter is 1 ~ 5 micron.
Carry out XRD diffraction to described pearl white, result shows, product prepared by the present invention is bismuth oxychloride crystals.
Embodiment 3
Bismuth chloride is dissolved in nitric acid, prepares the bismuth mixed salt solution that bismuth concentration is 2.1mol/L.
In the reaction vessel of 5L, add 1.5L deionized water, open and stir and add hydrochloric acid, adjust ph is 1.0, and above-mentioned mixing solutions is heated to 60 DEG C, adds 0.33g sorbester p18, under the condition of constant temperature, to the above-mentioned bismuth mixed salt solution of the mixed solution and dripping adding sorbester p18, rate of addition is 0.02ml/min, and slowly adds 6mol/LNaOH solution simultaneously and keep pH value to be 1.0.After 10 hours, stop adding bismuth mixed salt solution, continue to add NaOH solution, until reaction mixture pH value is 9.0, stops heating and stir, being down to room temperature, after filtering with distilled water wash, obtaining bismuth oxychloride crystals.
Carry out sem observation to pearl white, result is the pearl white scanning electron microscope diagram of preparation in the embodiment of the present invention 3 see Fig. 4, Fig. 4, and as shown in Figure 4, products therefrom presents tetragon or octagon thin plate crystal, and particle diameter is 1 ~ 5 micron.
Carry out XRD diffraction to described pearl white, result shows, product prepared by the present invention is bismuth oxychloride crystals.
Embodiment 4
Bismuth chloride is dissolved in nitric acid, prepares the bismuth mixed salt solution that bismuth concentration is 2.5mol/L.
In the reaction vessel of 5L, add 1.5L deionized water, open and stir and add hydrochloric acid, adjust ph is 3.0, and above-mentioned mixing solutions is heated to 70 DEG C, adds 0.8g oleyl amine, under the condition of constant temperature, to the above-mentioned bismuth mixed salt solution of the mixed solution and dripping adding oleyl amine, rate of addition is 0.04ml/min, and slowly adds 6mol/LNaOH solution simultaneously and keep pH value to be 3.0.After 12 hours, stop adding bismuth mixed salt solution, continue to add NaOH solution, until reaction mixture pH value is 10.0, stops heating and stir, being down to room temperature, after filtering with distilled water wash, obtaining pearl white.
Carry out sem observation to pearl white, result is the pearl white scanning electron microscope diagram of preparation in the embodiment of the present invention 4 see Fig. 5, Fig. 5, and as shown in Figure 5, products therefrom presents irregular thin plate crystal, and particle diameter is 8 ~ 15 microns.
Carry out XRD diffraction to described pearl white, result shows, product prepared by the present invention is bismuth oxychloride crystals.
Embodiment 5
Bismuth chloride is dissolved in nitric acid, prepares the bismuth mixed salt solution that bismuth concentration is 2.0mol/L.
In the reaction vessel of 5L, add 1.5L deionized water, open and stir and add hydrochloric acid, adjust ph is 4.0, and above-mentioned mixing solutions is heated to 85 DEG C, adds 0.7g fatty alcohol-polyoxyethylene ether, under the condition of constant temperature, to the above-mentioned bismuth mixed salt solution of the mixed solution and dripping adding fatty alcohol-polyoxyethylene ether, rate of addition is 0.05ml/min, and slowly adds 6mol/LNaOH solution simultaneously and keep pH value to be 4.0.After 10 hours, stop adding bismuth mixed salt solution, continue to add NaOH solution, until reaction mixture pH value is 9.0, stops heating and stir, being down to room temperature, after filtering with distilled water wash, obtaining bismuth oxychloride crystals.
Carry out sem observation to pearl white, result is the pearl white scanning electron microscope diagram of preparation in the embodiment of the present invention 5 see Fig. 6, Fig. 6, and as shown in Figure 6, products therefrom presents tetragon or octagon thin plate crystal, and particle diameter is 2 ~ 5 microns.
Carry out XRD diffraction to described pearl white, result shows, product prepared by the present invention is bismuth oxychloride crystals.
Embodiment 6
Bismuth chloride is dissolved in nitric acid, prepares the bismuth mixed salt solution that bismuth concentration is 2.4mol/L.
In the reaction vessel of 5L, add 1.5L deionized water, open and stir and add hydrochloric acid, adjust ph is 1.5, and above-mentioned mixing solutions is heated to 80 DEG C, adds 0.6g polyoxyethylene glycol, under the condition of constant temperature, to the above-mentioned bismuth mixed salt solution of the mixed solution and dripping adding polyoxyethylene glycol, rate of addition is 0.04ml/min, and slowly adds 6mol/LNaOH solution simultaneously and keep pH value to be 1.5.After 10 hours, stop adding bismuth mixed salt solution, continue to add NaOH solution, until reaction mixture pH value is 9.5, stops heating and stir, being down to room temperature, after filtering with distilled water wash, obtaining bismuth oxychloride crystals.
Carry out sem observation to pearl white, result is the pearl white scanning electron microscope diagram of preparation in the embodiment of the present invention 6 see Fig. 7, Fig. 7, and as shown in Figure 7, products therefrom presents quadrilateral thin plate crystal, and particle diameter is 2 ~ 5 microns.
Carry out XRD diffraction to described pearl white, result shows, product prepared by the present invention is bismuth oxychloride crystals.
Embodiment 7
Bismuth chloride is dissolved in nitric acid, prepares the bismuth mixed salt solution that bismuth concentration is 2.5mol/L.
In the reaction vessel of 5L, add 1.5L deionized water, open and stir and add hydrochloric acid, adjust ph is 3.5, and above-mentioned mixing solutions is heated to 85 DEG C, adds 0.4g polyvinyl alcohol, under the condition of constant temperature, to the above-mentioned bismuth mixed salt solution of the mixed solution and dripping adding polyvinyl alcohol, rate of addition is 0.05ml/min, and slowly adds 6mol/LNaOH solution simultaneously and keep pH value to be 3.5.After 12 hours, stop adding bismuth mixed salt solution, continue to add NaOH solution, until reaction mixture pH value is 10.0, stops heating and stir, being down to room temperature, after filtering with distilled water wash, obtaining bismuth oxychloride crystals.
Carry out sem observation to pearl white, result is the pearl white scanning electron microscope diagram of preparation in the embodiment of the present invention 7 see Fig. 8, Fig. 8, and as shown in Figure 8, products therefrom presents quadrilateral thin plate crystal, and particle diameter is 10 ~ 15 microns.
Carry out XRD diffraction to described pearl white, result shows, product prepared by the present invention is bismuth oxychloride crystals.
Above the preparation method of a kind of pearl white provided by the present invention is described in detail.Apply a concrete example herein to set forth principle of the present invention and embodiment, the explanation of above embodiment just understands method of the present invention and core concept thereof for helping.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improve and modify and also fall in the protection domain of the claims in the present invention.
Claims (6)
1. a preparation method for pearl white, comprises the following steps:
A1) hydrochloric acid and deionized water are mixed, obtain mixing solutions;
A2) in described mixing solutions, add nonionogenic tenside, then add bismuth mixed salt solution and react, add NaOH solution while adding bismuth mixed salt solution and keep reaction mixture pH value constant, after reaction, obtain bismuth oxychloride crystals; Described bismuth mixed salt solution comprises bismuth ion, chlorion, nitrate ion and water;
The quality of described nonionogenic tenside and the volume ratio of deionized water are (0.5 ~ 1.5g): 1L;
The rate of addition of described bismuth mixed salt solution is 0.02 ~ 0.06ml/min;
Described bismuth mixed salt solution is that Bismuth trinitrate is dissolved in hydrochloric acid, bismuth chloride is dissolved in nitric acid and bismuth oxide is dissolved in the mixed solution of nitric acid and hydrochloric acid one or more;
In described bismuth mixed salt solution, the concentration of bismuth ion is 1.5 ~ 2.5mol/L.
2. preparation method according to claim 1, is characterized in that, described constant pH is 0.1 ~ 4.0.
3. preparation method according to claim 1, it is characterized in that, described nonionogenic tenside be in OP emulsifying agent, tween emulsifier type, oleyl amine, fatty alcohol-polyoxyethylene ether, spans emulsifying agent, polyoxyethylene glycol, oleic acid and polyvinyl alcohol one or more.
4. preparation method according to claim 1, is characterized in that, the temperature of described reaction is 60 ~ 85 DEG C, and the time of described reaction is 10 ~ 20 hours.
5. preparation method according to claim 1, is characterized in that, described steps A 2) also comprise before:
By described steps A 1) mixing solutions that obtains is heated to 60 ~ 85 DEG C.
6. preparation method according to claim 1, is characterized in that, described steps A 2) be specially:
A21) in described mixing solutions, add nonionogenic tenside, then drip bismuth mixed salt solution and react, drip NaOH solution while adding bismuth mixed salt solution and keep reaction mixture pH value constant;
A22) after bismuth mixed salt solution dropwises, continue to add NaOH solution to reaction mixture, until reaction mixture pH value is 8.0 ~ 11.0 rear stopped reaction, obtain bismuth oxychloride crystals.
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| CN105214694B (en) * | 2015-09-30 | 2017-10-10 | 南京大学 | A kind of method that soft template method prepares BiOCl hollow shells |
| CN109077941B (en) * | 2018-07-13 | 2021-05-14 | 福建坤彩材料科技股份有限公司 | Colored bismuth oxychloride pigment and preparation method and application thereof |
| CN108910946B (en) * | 2018-10-10 | 2020-10-02 | 梁伟文 | Preparation method of oxidation-resistant bismuth oxychloride crystal |
| CN110624576A (en) * | 2019-10-14 | 2019-12-31 | 哈尔滨师范大学 | Preparation method of BiOCl photocatalyst with super-strong degradation effect |
| CN112850649B (en) * | 2020-12-29 | 2022-03-25 | 杭州电子科技大学 | Preparation method of bismuth oxybromide nanosheet |
| CN113649029B (en) * | 2021-08-18 | 2023-12-12 | 吉林建筑大学 | Preparation method and application of BiOCl nano photocatalyst with high visible light catalytic activity |
| CN114887633B (en) * | 2022-05-04 | 2024-02-02 | 宜春学院 | Uniform carbon modified ultrathin bismuth oxychloride photocatalyst and preparation method thereof |
| CN115364873A (en) * | 2022-08-22 | 2022-11-22 | 电子科技大学长三角研究院(湖州) | Hollow tubular ultrathin photocatalyst and preparation method thereof |
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