CN102943280B - A kind of method of electrochemical production Two-step purifying body - Google Patents
A kind of method of electrochemical production Two-step purifying body Download PDFInfo
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Abstract
The invention discloses a kind of method of electrochemical production Two-step purifying body, the method adopts high-purity aluminium sheet in the electrolyte solution of purifying after electrolysis, its electrolysate is obtained Two-step purifying body through high purity water washing, hydrothermal treatment consists, washing, drying, and its purity range is 99.9% ~ 99.999%.The inventive method gained has the Two-step purifying body of good dispersion, and its preparation technology is simple, and productive rate is high, and product stability is good; Environmentally safe, is easy to large-scale production.Two-step purifying body prepared by the present invention is widely used in multiple fields such as chemical industry, coating, building, traffic and electrical equipment.
Description
Technical field
The present invention relates to a kind of method of electrochemical production Two-step purifying body.
Background technology
High purity aluminium hydroxide is the ultrafine powder product that a kind of added value is very high, and its purity is 99.9% ~ 99.999%.It can as the whitening agent of papermaking filler, paper and optical brightener, the flocculation agent etc. of the fire-retardant filler such as rubber, resin, Urban water supply can also be applied to, be widely used in multiple fields such as chemical industry, coating, building, traffic and electrical equipment as a kind of new function material and structured material at present.High purity aluminium hydroxide is as inorganic combustion inhibitor in recent years, and its application makes substantial progress, and has become the fire retardant kind that application quantity is maximum in the world at present.But the technology of preparing relative progress of high purity aluminium hydroxide is slow, still there is numerous technical barrier, cause product performance unstable, the control of product purity is more difficult.
Through finding the literature search of prior art, the method preparing high purity aluminium hydroxide at present has multiple, as existing patent and literature procedure are mainly kind of a point-score, carbon method and sluggish precipitation etc.These methods respectively have feature, and aforesaid method all exists that control that is as too high in raw material preparation cost, particle size is more difficult, complex operation, have the problem demanding prompt solutions such as pollution to environment.As a kind of high pure and ultra-fine material of functionalization, the industrialized difficulty of preparation technology of high purity aluminium hydroxide is comparatively large, only has minority overseas enterprise can large-scale production at present.In view of this, special proposition the present invention.
Summary of the invention
In order to overcome the shortcoming that above-mentioned prior art exists, the invention provides that a kind of cost is low, experiment condition is simple, environmentally safe, being easy to the preparation method of the high purity aluminium hydroxide of suitability for industrialized production.
The technical scheme that technical solution problem of the present invention is taked is as follows: described preparation method be using surface treatment after high-purity aluminium sheet in negative electrode and anode electrolytic solution after purification, carry out electrolytic reaction simultaneously, gained electrolysate is obtained Two-step purifying body after washing, hydrothermal treatment consists, washing, drying.
In the technical scheme of above-mentioned preparation method: described raw material aluminium adopts high-purity aluminium sheet, purity is 99.99% ~ 99.999%.
In the technical scheme of above-mentioned preparation method: described surface treatment is: high-purity surface of aluminum plate first utilizes caustic dip, and then utilize lower concentration mineral acid washes.Wherein, described mineral acid is selected from the one in hydrochloric acid, nitric acid and sulfuric acid, and its concentration range is 0.05 ~ 0.5mol/L; Alkali lye is selected from the one in sodium hydroxide, potassium hydroxide, and its concentration range is 0.5 ~ 2.5g/L.
In preparation method of the present invention, effective constituent in the electrolytic solution that described electrolytic reaction adopts is the cats product of carbon atom number 5 ~ 25, and described tensio-active agent is any one in choline chloride 60, benzyl trimethyl ammonium chloride, Beta-methyl choline chloride 60, benzyltriethylammoinium chloride, benzyl dimethyl four decyl ammonium chloride.
In preparation method of the present invention, the purification process of described electrolytic solution is: with the electrolyte solution of high purity water preparation 50 ~ 500g/L, surface treated high-purity aluminium sheet is that anode and cathode carries out electrolysis and by electrolysate filtering separation, filtrate is for subsequent use as the electrolytic solution after purifying.
In preparation method of the present invention, described electrolytic reaction adopts power supply to be direct supply.
In preparation method of the present invention, described electrolysis in pH6 ~ 10, current density 1 ~ 5A/dm
2, temperature 30 ~ 90 DEG C, mechanical stirring or pneumatic blending gas pushing quantity are carry out under the condition of 100 ~ 3000L/min.
In electrolytic reaction of the present invention, when the content of electrolysate in electrolytic solution and white aluminium hydroxide powder is 3% ~ 30%, be separated by electrolyte filtering, as passed through dynamic separation aluminium hydroxide powder, namely filtrate use as the circulation of elecrolyte of purifying of the present invention.In this step, the separation method that the separation of electrolysate adopts those skilled in the art usual.
In preparation method of the present invention, described hydrothermal treatment consists is: electrolysate is put into high pressure vessel, and add high purity water, crystal seed and organic anion, be 100 ~ 300 DEG C in temperature, pressure is that under the condition of 1 ~ 87kg, constant temperature 1 ~ 48h carries out hydrothermal treatment consists; Wherein, the consumption of high purity water is 1 ~ 8 times of aluminium hydrate powder body weight; The consumption of organic anion is 0.5 ‰ ~ 10% of aluminium hydrate powder body weight.
In above-mentioned hydrothermal treatment consists, described crystal seed is the Two-step purifying body of particle diameter 5 ~ 100nm, and its injected volume is aluminium hydrate powder body weight 1 ‰ ~ 10%.
In preparation method of the present invention, described organic anion is the one in tartrate or citric acid.
In preparation method of the present invention, described washing, refer to that the aluminium hydroxide powder high purity water after by hydrothermal treatment consists washs, this bath water can recycle after treatment.
In preparation method of the present invention, the electrical resistivity range of described high purity water is 10 ~ 18.3M Ω .cm.
As a kind of preferred forms of the present invention, the present invention preferably adopts following preparation method: high-purity aluminium sheet is carried out surface treatment, and is the purifying electrolytic solution of 400g/L containing benzyl trimethyl ammonium chloride amount.High-purity aluminium sheet after surface treatment is placed in the electrolytic solution after purifying, in pH8 ~ 10 as negative electrode and anode simultaneously; Current density 1A/dm
2, temperature is 50 DEG C, and pneumatic blending gas pushing quantity is electrolysis aluminium sheet under the condition of 100L/min.When powder content reaches 25% in electrolytic solution, after filtering tank liquor, obtain aluminium hydroxide powder; By aluminium hydroxide powder after high purity water washing, putting into high pressure vessel, and add the tartrate of high purity water, crystal seed and aluminium hydrate powder body weight 5%, is 150 DEG C in temperature, and pressure is constant temperature 1h under the condition of 30kg.Take out aluminium hydroxide powder through washing, after drying, Two-step purifying body can be obtained.
Adopt technique scheme, the purity range of high purity aluminium hydroxide prepared by the present invention is 99.99% ~ 99.999%, and yield is 40% ~ 90%.
Compared to existing technology, the present invention has following beneficial effect:
1. the Two-step purifying body of preparation, its purity range is 99.9% ~ 99.999%, and yield is 40% ~ 90%.
2. in Two-step purifying production procedure, agents useful for same is the organic composition that volatility is little, not containing inorganic additive, also can not introduce impurity element simultaneously, highly beneficial to preparing high purity product.
3. in Two-step purifying production procedure, high purity water used can be recycled, without a large amount of waste residue, waste gas and discharge of wastewater, extremely beneficial to environment protection, belongs to environment-friendly type technique.
4. preparation technology of the present invention is simple, and production cost is lower, and scale and benefit are strong, easy to utilize.
Embodiment
Embodiment 1
The preparation method of the high purity aluminium hydroxide of present embodiment carries out in accordance with the following steps: high-purity aluminium sheet is carried out surface treatment, and purifying chloride containing choline amount is the electrolytic solution of 200g/L.High-purity aluminium sheet after surface treatment is placed in the electrolytic solution after purifying as negative electrode and anode simultaneously, and be 7 ~ 8 at pH, current density is 3A/dm
2, temperature is 60 DEG C, and mechanical stirring gas pushing quantity is electrolysis aluminium sheet under the condition of 800L/min.When levels of precipitate reaches 28% in electrolytic solution, after filtering tank liquor, obtain aluminium hydroxide powder; By aluminium hydroxide powder after washing, put into high pressure vessel, and add the citric acid of high purity water, crystal seed and filter cake weight 5%; Temperature be 200 DEG C, pressure be the condition of 12kg under constant temperature 6h carry out hydrothermal treatment consists; Wherein the consumption of high purity water is 4 times of aluminium hydrate powder body weight; Described crystal seed is the nano-aluminum hydroxide powder of particle diameter 50nm, and its injected volume is aluminium hydrate powder body weight 5%; Tartaric consumption is 6% of aluminium hydrate powder body weight.Take out after hydrothermal treatment consists through washing, after drying, Two-step purifying body can be obtained.
Through above-mentioned preparation process, the purity of the Two-step purifying body finally obtained is 99.95%, and yield is 70%.
Embodiment 2
The preparation method of the high purity aluminium hydroxide of present embodiment carries out in accordance with the following steps:
High-purity aluminium sheet is carried out surface treatment, and purifying is the electrolytic solution of 400g/L containing benzyl trimethyl ammonium chloride amount.High-purity aluminium sheet after surface treatment is placed in the electrolytic solution after purifying, in pH8 ~ 10 as negative electrode and anode simultaneously; Current density 1A/dm
2, temperature is 40 DEG C, and mechanical stirring gas pushing quantity is electrolysis aluminium sheet under the condition of 100L/min.When levels of precipitate reaches 15% in electrolytic solution, after filtering tank liquor, obtain aluminium hydroxide powder; By aluminium hydroxide powder after washing, putting into high pressure vessel, and add the citric acid of high purity water, crystal seed and aluminium hydrate powder body weight 5%, is 100 DEG C in temperature, and pressure is that under the condition of 10kg, constant temperature 1h carries out hydrothermal treatment consists; Wherein the consumption of high purity water is 3 times of aluminium hydrate powder body weight; Described crystal seed is the nano-aluminum hydroxide powder of particle diameter 5nm, and its injected volume is aluminium hydrate powder body weight 1 ‰; The consumption of citric acid is 6% of aluminium hydrate powder body weight.Take out after hydrothermal treatment consists through washing, after drying, Two-step purifying body can be obtained.
The purity of Two-step purifying body prepared by the present embodiment is 99.99%, and yield is 80%.
Embodiment 3
The preparation method of the high purity aluminium hydroxide of present embodiment carries out in accordance with the following steps:
High-purity aluminium sheet is carried out surface treatment, and purifying is the electrolytic solution of 400g/L containing benzyltriethylammoinium chloride amount.High-purity aluminium sheet after surface treatment is placed in the electrolytic solution after purifying, in pH8 ~ 10 as negative electrode and anode simultaneously; Current density 5A/dm
2; Temperature is 90 DEG C; Pneumatic blending gas pushing quantity is electrolysis aluminium sheet under the condition of 1000L/min.When aluminium hydrate powder body burden reaches 30% in electrolytic solution, after being filtered by tank liquor, obtain aluminium hydroxide powder; After being washed by aluminium hydroxide powder, putting into high pressure vessel, and add the tartrate of high purity water, crystal seed and aluminium hydrate powder body weight 10%, is 300 DEG C in temperature; Pressure is that under the condition of 87kg, constant temperature 30h carries out hydrothermal treatment consists; Wherein the consumption of high purity water is 5 times of aluminium hydrate powder body weight; Described crystal seed is the nano-aluminum hydroxide powder of particle diameter 100nm, and its injected volume is aluminium hydrate powder body weight 10%; Tartaric consumption is 2% of aluminium hydrate powder body weight.Take out after hydrothermal treatment consists through high purity water washing, after drying, Two-step purifying body can be obtained.
The purity of Two-step purifying body prepared by the present embodiment is 99.995%, and yield is 75%.
Embodiment 4
The preparation method of the high purity aluminium hydroxide of present embodiment carries out in accordance with the following steps:
High-purity aluminium sheet is carried out surface treatment, and purifying chloride containing choline amount is the electrolytic solution of 50g/L.High-purity aluminium sheet after surface treatment is placed in the electrolytic solution after purifying as negative electrode and anode simultaneously, in pH7 ~ 8, current density 3A/dm
2, temperature is 60 DEG C, and pneumatic blending gas pushing quantity is electrolysis aluminium sheet under the condition of 3000L/min.When levels of precipitate reaches 3% in electrolytic solution, after filtering tank liquor, obtain aluminium hydroxide powder; By aluminium hydroxide powder after washing, putting into high pressure vessel, and add high purity water, crystal seed and tartrate, is 200 DEG C in temperature, and pressure is that under the condition of 32kg, constant temperature 24h carries out hydrothermal treatment consists; Wherein, the consumption of high purity water is 8 times of aluminium hydrate powder body weight; Described crystal seed is the nano-aluminum hydroxide powder of particle diameter 20nm, and its injected volume is aluminium hydrate powder body weight 5%; Tartaric consumption is 0.5 ‰ of aluminium hydrate powder body weight.Take out after hydrothermal treatment consists, through high purity water washing, after drying, Two-step purifying body can be obtained.
The purity of Two-step purifying body prepared by the present embodiment is 99.995%, and yield is 70%.
Embodiment 5
The preparation method of the high purity aluminium hydroxide of present embodiment carries out in accordance with the following steps:
High-purity aluminium sheet is carried out surface treatment, and purifying is the electrolytic solution of 500g/L containing benzyl dimethyl four decyl ammonium chloride amount.High-purity aluminium sheet after surface treatment is placed in the electrolytic solution after purifying as negative electrode and anode simultaneously, in pH6 ~ 7, current density 5A/dm
2, temperature is 30 DEG C, and mechanical stirring gas pushing quantity is electrolysis aluminium sheet under the condition of 2000L/min.When levels of precipitate reaches 10% in electrolytic solution, after filtering tank liquor, obtain aluminium hydroxide powder; By aluminium hydroxide powder after washing, putting into high pressure vessel, and add high purity water, crystal seed and citric acid, is 150 DEG C in temperature, and pressure is that under the condition of 7kg, constant temperature 48h carries out hydrothermal treatment consists; Wherein, the consumption of high purity water is 1 times of aluminium hydrate powder body weight; Described crystal seed is the nano-aluminum hydroxide powder of particle diameter 30nm, and its injected volume is aluminium hydrate powder body weight 1%; The consumption of citric acid is 5% of aluminium hydrate powder body weight.Take out after hydrothermal treatment consists, through high purity water washing, after drying, Two-step purifying body can be obtained.
The purity of Two-step purifying body prepared by the present embodiment is 99.95%, and yield is 40%.
Embodiment 6
The preparation method of the high purity aluminium hydroxide of present embodiment carries out in accordance with the following steps:
High-purity aluminium sheet is carried out surface treatment, and purifying is the electrolytic solution of 400g/L containing Beta-methyl choline chloride 60.High-purity aluminium sheet after surface treatment is placed in the electrolytic solution after purifying as negative electrode and anode simultaneously, in pH8 ~ 10, current density 5A/dm
2, temperature is 30 DEG C, and mechanical stirring gas pushing quantity is electrolysis aluminium sheet under the condition of 100L/min.When levels of precipitate reaches 20% in electrolytic solution, after filtering tank liquor, obtain aluminium hydroxide powder; By aluminium hydroxide powder after washing, putting into high pressure vessel, and add high purity water, crystal seed and tartrate, is 100 DEG C in temperature, and pressure is that under the condition of 37kg, constant temperature 48h carries out hydrothermal treatment consists; Wherein, the consumption of high purity water is 2 times of aluminium hydrate powder body weight; Described crystal seed is the nano-aluminum hydroxide powder of particle diameter 60nm, and its injected volume is aluminium hydrate powder body weight 7%; Tartaric consumption is 10% of aluminium hydrate powder body weight.Take out after hydrothermal treatment consists, through high purity water washing, after drying, Two-step purifying body can be obtained.
The purity of Two-step purifying body prepared by the present embodiment is 99.99%, and yield is 75%.
Embodiment in above-described embodiment can combine further or replace; and embodiment is only be described the preferred embodiments of the present invention; not the spirit and scope of the present invention are limited; under the prerequisite not departing from design philosophy of the present invention; the various changes and modifications that in this area, professional and technical personnel makes technical scheme of the present invention, all belong to protection scope of the present invention.
Claims (7)
1. the preparation method of a high purity aluminium hydroxide, it is characterized in that, described preparation method be using surface treatment after high-purity aluminium sheet in the electrolytic solution of purifying, carry out electrolytic reaction as negative electrode and anode simultaneously, gained electrolysate is obtained Two-step purifying body after washing, hydrothermal treatment consists, washing, drying; The effective constituent of described electrolytic solution is the cats product of carbon atom number 5 ~ 25, and described tensio-active agent is any one in choline chloride 60, benzyl trimethyl ammonium chloride, Beta-methyl choline chloride 60, benzyltriethylammoinium chloride, benzyl dimethyl four decyl ammonium chloride; Described hydrothermal treatment consists is: put into high pressure vessel after being filtered by electrolysate aluminium hydroxide powder, and add high purity water, crystal seed and organic anion, be 100 ~ 300 DEG C in temperature, pressure is that under the condition of 1 ~ 87kg, constant temperature 1 ~ 48h carries out hydrothermal treatment consists; Wherein, described organic anion is the one in tartrate or citric acid, and the consumption of high purity water is 1 ~ 8 times of aluminium hydrate powder body weight; The consumption of organic anion is 0.5 ‰ ~ 10% of aluminium hydrate powder body weight; Described crystal seed is the nano-aluminum hydroxide powder of particle diameter 5 ~ 100nm, and the injected volume of crystal seed is 1 ‰ ~ 10% of aluminium hydrate powder body weight.
2. preparation method according to claim 1, it is characterized in that, the preparation method of electrolyte of described purifying is as follows: with the electrolyte solution of high purity water preparation 50 ~ 500g/L, surface treated high-purity aluminium sheet is that anode and cathode carries out electrolysis and by electrolysate filtering separation, filtrate is for subsequent use as the electrolytic solution after purifying.
3. preparation method according to claim 1, is characterized in that, described electrolytic reaction adopts power supply to be direct supply.
4. preparation method according to claim 1, is characterized in that, described electrolytic reaction in pH6 ~ 10, current density 1 ~ 5A/dm
2, temperature is 30 ~ 90 DEG C, and mechanical stirring or pneumatic blending gas pushing quantity are carry out under the condition of 100 ~ 3000L/min.
5. preparation method according to claim 1, is characterized in that, when in electrolytic solution, the content of electrolysate white aluminium hydroxide powder is 3% ~ 30%, be separated by electrolyte filtering, filtrate is for subsequent use as the electrolytic solution after purifying.
6. preparation method according to claim 1, is characterized in that, the electrical resistivity range of described high purity water is 10 ~ 18.3M Ω cm.
7. preparation method according to claim 1, it is characterized in that, described preparation method is: high-purity aluminium sheet is carried out surface treatment, and contain the purifying electrolytic solution that benzyl trimethyl ammonium chloride amount is 400g/L, high-purity aluminium sheet after surface treatment is placed in the electrolytic solution after purifying, in pH8 ~ 10 as negative electrode and anode simultaneously; Current density 1A/dm
2, temperature is 30 DEG C, and pneumatic blending gas pushing quantity is electrolysis aluminium sheet under the condition of 100L/min, when solids content reaches 25% in electrolytic solution, obtains aluminium hydroxide powder after filtering tank liquor; By aluminium hydroxide powder after washing, putting into high pressure vessel, and add the tartrate of high purity water, crystal seed and aluminium hydrate powder body weight 5%, is 100 DEG C in temperature, and pressure is constant temperature 1h under the condition of 30kg; Take out through high purity water washing, after drying, Two-step purifying body can be obtained.
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| CN104047015B (en) * | 2014-06-19 | 2017-02-01 | 郑州昆研新材料科技有限公司 | Method for preparing high-purity alumina powder by alternating current electrolysis |
| CN108217705A (en) * | 2016-12-10 | 2018-06-29 | 中国科学院大连化学物理研究所 | A kind of preparation method of alumina in Nano level |
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