CN109534396A - A kind of transition state sb oxide and preparation method thereof - Google Patents
A kind of transition state sb oxide and preparation method thereof Download PDFInfo
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- CN109534396A CN109534396A CN201811603920.7A CN201811603920A CN109534396A CN 109534396 A CN109534396 A CN 109534396A CN 201811603920 A CN201811603920 A CN 201811603920A CN 109534396 A CN109534396 A CN 109534396A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G30/00—Compounds of antimony
- C01G30/004—Oxides; Hydroxides; Oxyacids
- C01G30/005—Oxides
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/30—Three-dimensional structures
- C01P2002/36—Three-dimensional structures pyrochlore-type (A2B2O7)
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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Abstract
The present invention relates to acidic bodies of water cleanser preparation fields, and to solve in the prior art there has been no the method that one kind can quickly and easily prepare high activity sb oxide cleanser, the present invention provides a kind of transition state sb oxides and preparation method thereof.Comprising: 1) weighed and be mixed to prepare mixed solution using antimony trichloride and hydrochloric acid as raw material；2) excessive chlorine is passed through into mixed solution to be reacted；3) mixed solution is added into a large amount of water and is hydrolyzed, and hydrolysate is allowed to be aged in hydrolysising mother liquid, crystalline state sb oxide is obtained by filtration；4) crystalline state sb oxide is calcined, obtains transition state sb oxide.The method of the present invention simple process can prepare the transition state sb oxide of high mesh number high activity；Obtained transition state sb oxide, which is used to remove arsenic, antimony, bismuth in acidic bodies of water, has good using effect；Efficiency of pcr product is high, and reaction is controllable；The recyclable recycling such as hydrochloric acid, water in reaction process.
Description
Technical field
The present invention relates to acidic bodies of water cleanser preparation field more particularly to a kind of transition state sb oxide and its preparation sides
Method.
Background technique
Antimony can form a series of antimony oxygen compound, such as Sb in conjunction with oxygen2O5、Sb6O13、Sb2O4、Sb2O3、SbO2、Sb2O
And gaseous state SbO etc..Wherein Sb2O5And Sb2O3It is furtherd investigate and is widely applied.Both sb oxides can be made
It is industrial that enamel, rubber, plastics and dyeing and weaving etc. are widely used in for the multiple agent of screening, filler and catalyzer contact agent etc..But in Patent Office of the People's Republic of China
A kind of entitled method of copper electrolyte precipitation to remove impurities, Publication No. CN107164786A disclosed on September 15th, 2017
Sb oxide is described in application for a patent for invention in acidic bodies of water (copper electrolyte is acidity) for going arsenic removal antimony bismuth etc. several
The effect of toxic and harmful element, and in Xiao F X, Cao D, Mao J W, et al.Role of Sb (V) in
removal of As,Sb and Bi impurities from copper electrolyte[J].Transactions of
Nonferrous Metals Society of China, 2014,24 (1): has further stated that Sb in mono- text of 271-278.2O5
Excellent effect when removing harmful element arsenic antimony bismuth for acidic bodies of water.Therefore, antimony pentoxide is as a kind of acidic bodies of water
Cleanser is the research direction for the prospect that is rich in.
But at present merely with pentavalent sb oxide and its hydrate (antimony pentoxide/Sb2O5/Sb2O5·nH2O) make
It is extremely limited for the cleanser using effect of acidic bodies of water.This is limited to the high stability of antimony pentoxide crystal, in water body
Solubility it is extremely limited.In addition, existing pentavalent sb oxide is generally by ion-exchange, reflux oxidation method, chlorine antimony
The preparation of the methods of sour water solution ammonification precipitating, potassium antimonate/sodium antimonate sol-gel process.Preparation process is relatively complicated, and obtained
Quinquevalence antimony oxide particle is larger, usually in the micron-scale more than above (>=1 μm).Then specific surface area is small greatly for its partial size, causes
It is relatively low with the touch opportunity of the foreign ion in acidic bodies of water, and the absorption played, reaction co-precipitation and other effects are poor.
In this regard, Patent Office of the People's Republic of China also disclosed a kind of solution atomization method on July 14th, 2017 prepares ultra-fine sb oxide
Method invention patent mandate, authorize Publication No. CN105858724B comprising following steps: (1) trivalent antimony is added
The antimony solution of 0.05~0.8mol/L is configured into hydrochloric acid solution；(2) oxygen is carried out to step (1) solution using cleaning oxidizer
Change, obtains quinquevalence antimony solution；(3) the quinquevalence antimony solution that step (2) obtains is subjected to atomization pyrolysis, obtains thinner sb oxide powder
End.It is only micron particles by sb oxide obtained by oxidation and spray pyrolysis but in the inventive technique scheme, and
And it can only prepare the pentavalent sb oxide of single valence.In addition, dispersibility is poor when spray pyrolysis, crystal coarsening rate compared with
Fastly, the activity of pentavalent sb oxide is to be improved.
Summary of the invention
To solve the problems, such as that there has been no the method that one kind can prepare high activity pentavalent sb oxide, this hairs in the prior art
It is bright to provide a kind of transition state sb oxide and preparation method thereof.It first has to the mesh for realizing preparation high mesh number pentavalent sb oxide
, and the transition state sb oxide of high activity is prepared on this basis, sb oxide is improved as acidic bodies of water water purification agent
Purifying water effect when use.
To achieve the above object, the present invention uses following technical scheme.
A kind of preparation method of transition state sb oxide, the preparation method includes following preparation step:
1) using antimony trichloride and hydrochloric acid as raw material, weighed and be mixed to prepare mixed solution；
2) it is passed through excessive chlorine into mixed solution and carries out oxidation reaction；
3) solution after reaction is added into a large amount of water and is hydrolyzed, and hydrolysate is allowed to be aged in hydrolysising mother liquid, filtered
Obtain crystalline state pentavalent sb oxide；
4) crystalline state pentavalent sb oxide is calcined, obtains transition state sb oxide, i.e., with the pyrochlore-type of mixed valence
Sb oxide.
The method of the present invention selects the antimony trichloride being stabilized in a certain concentration hydrochloric acid molten as raw material preparation trivalent antimony
Liquid, trivalent antimony are in the solution quinquevalence antimony by chlorine oxidation, and then the Antimony pentachloride hydrochloric acid solution of formation is added to a large amount of water
Middle formation suspension.Concentrated hydrochloric acid can not inhibit Antimony pentachloride hydrolysis after diluting, therefore Antimony pentachloride hydrolyzes to form
Hydrous antimony pentoxide (HAP) simultaneously forms nano-sized crystalline hydrous antimony oxide S b in further ageing process2O5·4H2O.It is calcining
In the process, control calcination condition makes crystalline state hydration sb oxide lose the crystallization water.The hydration sb oxide of crystalline state starts simultaneously at hair
It is born from reduction reaction, form the transition state sb oxide containing part trivalent antimony and releases oxygen, being formed has compared with Gao Bibiao
The transition state sb oxide powder that area, partial size are about 60~120nm.Mole of quinquevalence antimony in resulting transition state sb oxide
Score is about 0.68~0.9, remaining is trivalent antimony.And due to losing for the formation of trivalent antimony and the crystallization water, transition state antimony oxygen
The crystal grain of compound is divided, destroys, and a large amount of defect and hole occurs in transition state sb oxide crystal grain, makes its large specific surface area
Width improves, and increases and the chance of the contact of foreign ion in acidic bodies of water.And due to the generation of a large amount of defects, in acidity
The antimony concentration in water body can be improved in water body in a short time, to realize in efficiently removal water body including arsenic antimony bismuth
The purpose of toxic heavy metal.
Preferably, the solid-to-liquid ratio of antimony trichloride and hydrochloric acid used in step 1) is 1kg:(2~4) L.
Due to antimony trichloride facile hydrolysis, it is therefore desirable to which more hydrochloric acid is to inhibit to hydrolyze.But hydrochloric acid dosage is excessive, is easy
It causes subsequent formulation to need to be added excessive water when forming hydrolysising mother liquid, results in waste of resources.Therefore, which is most
Good proportional region.
Preferably, hydrochloric acid used in step 1) is concentration >=20wt% concentrated hydrochloric acid.
The hydrochloric acid of low concentration can not inhibit antimony trichloride to hydrolyze to form trivalent antimony oxide precipitation in the solution, it is therefore desirable to
Concentrated hydrochloric acid, which hydrolyzes it, to be inhibited.
Preferably, hydrochloric acid used in step 1) is concentration >=36wt% concentrated hydrochloric acid.
The hydrochloric acid more than concentration range is more outstanding to the inhibitory effect of antimony trichloride.
Preferably, the molar ratio of antimony trichloride used in chlorine and step 1) that step 2) is passed through is (1.5~2.5):
1。
Excessive chlorine is passed through to guarantee that trivalent antimony can be fully oxidized as quinquevalence antimony, is aged and forges to avoid to subsequent
Burning process adversely affects.
It is hydrolyzed preferably, being added solution after the step 3) reaction into the water of its 70~100 times of volumes.
Enough water, which is added, can promote hydrolysis completely, if plus will lead to hydrolysis not exclusively if water is excessively few, hydrolyzate sheet
Body becomes the pollutant effluents containing antimony, then will lead to water resource waste with dilutional hyponatremia.And after complete hydrolysis and filtering, water can be located
It manages and recycles, reuse, it is environmentally protective.
Preferably, the step 3) hydrolysis temperature is 20~25 DEG C, digestion time is 5~7d.
Hydrolysis temperature is too low to will lead to hydrolyzed slow, reduction efficiency, and temperature is excessively high, will lead to the too fast shape of hydrolysis
At the biggish crystalline state sb oxide of partial size, the subsequent particle size being prepared is larger, and influences the autoreduction of calcination process
Reaction.In the temperature range, it can ensure that hydrolysis is complete in the digestion time.
Preferably, calcination temperature is 300~700 DEG C in the step 4) calcination process, calcination time is 5~6h.
At 300 DEG C or more, it is trivalent antimony that quinquevalence antimony, which starts autoreduction,.The quinquevalence antimony rate of reduction within the scope of 300~700 DEG C
Relatively slowly, controllability is stronger, and the autoreduction reaction rate in 700 DEG C or more quinquevalence antimonies increases substantially, it is difficult to which preparation is main
Using quinquevalence antimony as the transition state sb oxide of principal component, or even it is easy complete autoreduction and forms trivalent sb oxide (Sb2O3), it loses
Go it as the value of acidic bodies of water water purification agent.In addition, heat treatment temperature is excessively high, transition state sb oxide is easy to happen recrystallization
Behavior loses itself defect and hole.Prepared powder specific-surface area detection is reduced rapidly, and activity significantly reduces.
Preferably, calcination temperature is 300~400 DEG C in the step 4) calcination process, calcination time is 5~6h.
Slowly, controllably, formation at least contains 71atom% quinquevalence antimony to the rate of reduction of quinquevalence antimony within this temperature range
Transition state sb oxide when as acidic bodies of water water purification agent activity with higher.
Preferably, step 4) the calcination process heating rate is 5~10 DEG C/min.
Heating rate is too fast, and during will lead to quinquevalence antimony autoreduction production trivalent antimony, dehydration is not exclusively difficult to be formed scarce
It falls into, reduces clean-up effect.
A kind of transition state sb oxide, the molar percentage of quinquevalence antimony is 68~90% in the transition state sb oxide,
Remaining is trivalent antimony.
Crystal grain contained in transition state sb oxide is divided in forming process, destroys, therefore occurs in crystal grain a large amount of
Defect and hole, make it have higher specific surface area, increase and the chance of the contact of foreign ion in acidic bodies of water.And
And due to the generation of a large amount of defects, the antimony concentration in water body can be improved in a short time in acidic bodies of water, to realize
The efficiently purpose of the toxic heavy metal in removal water body including arsenic antimony bismuth.
The beneficial effects of the present invention are:
1) the method for the present invention simple process can prepare the transition state sb oxide of high mesh number；
2) there is high activity by the transition state sb oxide for being controllably heat-treated preparation；
3) products collection efficiency is high, and reaction is controllable；
4) the recyclable recycling such as the hydrochloric acid in reaction process, water.
Detailed description of the invention
Fig. 1 is that the TG/DTG of the embodiment of the present invention schemes；
Fig. 2 is the XRD testing result of the embodiment of the present invention；
Fig. 3 is the SEM of commercially available antimony pentoxide and the TEM figure of Examples 1 to 5；
Fig. 4 is the XPS spectrum figure of the embodiment of the present invention.
Specific embodiment
Further clear detailed description explanation is made to the present invention below in conjunction with specific embodiment and Figure of description.This
Field those of ordinary skill will realize the present invention based on these explanations.In addition, being related in following the description
The embodiment of the present invention be generally only an of the invention branch embodiment, instead of all the embodiments.Therefore, it is based on this hair
Embodiment in bright, those of ordinary skill in the art's every other reality obtained without making creative work
Example is applied, should fall within the scope of the present invention.
Unless otherwise specified, in the embodiment of the present invention it is raw materials used be commercially available or those skilled in the art obtained by original
Material；Unless otherwise specified, method therefor method known to those skilled in the art in the embodiment of the present invention.
Examples 1 to 5
A kind of preparation method of transition state sb oxide, the preparation method includes following preparation step:
1) using antimony trichloride and hydrochloric acid as raw material, weighed and be mixed to prepare mixed solution；
2) excessive chlorine is passed through into mixed solution to be reacted；
3) mixed solution is added into a large amount of water and is hydrolyzed, and hydrolysate is allowed directly to be aged in hydrolysising mother liquid, filtered
Obtain crystalline state sb oxide；
4) crystalline state sb oxide is calcined, obtains transition state sb oxide, that is, there is the pyrochlore constitution of mixed valence
Sb oxide detects obtained transition state sb oxide.
Wherein, the preparation parameter of Examples 1 to 5 and average droplet measurement result are as shown in following table Tables 1 and 2.
The specific preparation parameter of table 1 and average grain diameter testing result (I)
The specific preparation parameter of table 2 and average grain diameter testing result (II)
Again to transition state sb oxide obtained by Examples 1 to 5, and to be calcined within the scope of 100~800 DEG C through remaining
Sample after temperature calcination carries out every detection.Wherein, TG/DTG testing result is as shown in Figure 1.From figure it will be evident that
300 DEG C or less there is significant weightless peak, the antimony in 300 to 400 DEG C of calcination temperature ranges due to the removing DTG curve of the crystallization water
There is more gentle weightless process in oxide, this is because the removing of quinquevalence antimony autoreduction process oxygen atom causes.The temperature model
Enclose it is interior reaction it is the gentlest, controllability is most strong.And can be seen that from Fig. 2 XRD diagram, (111) are brilliant in antimony pentoxide at normal temperature
Face peak and (311) crystal face peak are higher, and (222) crystal face peak is more weak, but as calcination temperature reaches 300 DEG C or more, such as 350
DEG C when, apparent offset and Strength Changes occur for (111) crystal face peak, (222) crystal face peak and (311) crystal face peak, wherein (111) are brilliant
Face peak and (311) crystal face peak intensity obviously die down, and (222) crystal face peak is remarkably reinforced, and illustrates especially to exist after reaching 300 DEG C
350 DEG C or so, since quinquevalence antimony autoreduction is trivalent antimony, mother crystal structure is by large effect and destruction；It further increases
Sb can be changed into when calcination temperature6O13Phase, to lose activity.For another example SEM and TEM shown in Fig. 3 scheme, and a is commercially available five in Fig. 3
The SEM figure and pictorial diagram at two antimony powders end are aoxidized, b to f is the TEM figure for being respectively exemplified 1~5 in figure.It can be sent out from figure
Transition state sb oxide has more coarse particle surface and Jie abundant in present 300 to 400 DEG C of calcination temperature ranges
Pore structure, so transition state sb oxide specific surface area with higher at this time.And 700 DEG C of heat treatment temperature makes transition
State sb oxide is changed into Sb6O13Phase causes transition state sb oxide to lose crystal defect, active rapid decrease.Fig. 4 a is real
XPS figure of the transition state sb oxide obtained by example 3 at 60 DEG C after drying is applied, Fig. 4 b is the calcined transition state antimony of different temperatures
The XPS of oxide schemes.As we can see from the figure with the rising of calcination temperature, the trivalent antimony content in transition state sb oxide is not
It is disconnected to increase, gradually it is changed into the sb oxide with mixed valence of high activity；But after 700 DEG C of high-temperature calcinations, antimony oxidation
Although object has mixed valence feature, stable Sb is had turned to6O13Phase no longer has reactivity.
Soluble arsenic, soluble bismuth salt and soluble antimonic salt are dissolved in dilute sulfuric acid and are formulated as liquid to be processed, to survey
Try the activity and removal of impurities performance of prepared transition state sb oxide.Utilize transition state antimony oxygen obtained by above-described embodiment 1~5
Compound is added with the solid-to-liquid ratio of 20g/L into liquid to be processed, stirs 30min under the conditions of 60 DEG C, treat arsenic in treatment fluid, antimony,
Bismuth element content is detected, and testing result is as shown in table 3 below.
Table 3 is to arsenic, antimony, bismuth element removal rate result
From upper table it will be evident that by the comparison with business antimony pentoxide, transition state obtained by the method for the present invention
Sb oxide there is extremely excellent removal effect, especially antimony element can realize very the arsenic antimony bismuth in acidic bodies of water
Removal.
Claims (10)
1. a kind of preparation method of transition state sb oxide, which is characterized in that the preparation method includes following preparation step:
1) using antimony trichloride and hydrochloric acid as raw material, weighed and be mixed to prepare mixed solution；
2) it is passed through excessive chlorine into mixed solution and carries out oxidation reaction；
3) solution after reaction is added into a large amount of water and is hydrolyzed, and hydrolysate is allowed to be aged in hydrolysising mother liquid, filtered
Obtain crystalline state pentavalent sb oxide；
4) crystalline state sb oxide is calcined, obtains transition state sb oxide, that is, there is the pyrochlore constitution of mixed valence
Sb oxide.
2. a kind of preparation method of transition state sb oxide according to claim 1, which is characterized in that three used in step 1)
The solid-to-liquid ratio of antimony chloride and hydrochloric acid is 1kg:(2~4) L.
3. a kind of preparation method of transition state sb oxide according to claim 1 or 2, which is characterized in that step 1) institute
It is concentration >=20wt% concentrated hydrochloric acid with hydrochloric acid.
4. a kind of preparation method of transition state sb oxide according to claim 1, which is characterized in that step 2) is passed through
Chlorine and step 1) used in antimony trichloride molar ratio be (1.5~2.5): 1.
5. a kind of preparation method of transition state sb oxide according to claim 1, which is characterized in that step 3) is described mixed
Conjunction solution, which is added into the water of its 70~100 times of volumes, to be hydrolyzed.
6. a kind of preparation method of transition state sb oxide according to claim 1 or 5, which is characterized in that step 3) institute
State that hydrolysis temperature is 20~25 DEG C, digestion time is 5~7d.
7. a kind of preparation method of transition state sb oxide according to claim 1, which is characterized in that step 4) is described to forge
Calcination temperature is 300~700 DEG C during burning, calcination time is 5~6h.
8. a kind of preparation method of transition state sb oxide according to claim 1, which is characterized in that step 4) is described to forge
Calcination temperature is 300~400 DEG C during burning, calcination time is 5~6h.
9. a kind of preparation method of transition state sb oxide described according to claim 1 or 7 or 8, which is characterized in that step 4)
The calcination process heating rate is 5~10 DEG C/min.
10. a kind of transition state sb oxide as made from claim 1 to 9 any one the method, which is characterized in that described
The molar percentage of quinquevalence antimony is 68~90% in transition state sb oxide, remaining is trivalent antimony.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109988921A (en) * | 2019-04-17 | 2019-07-09 | 北京矿冶科技集团有限公司 | The method of antimony is separated in a kind of hydrochloric acid-chloride solution |
| CN110902720A (en) * | 2019-12-19 | 2020-03-24 | 新邵辰州锑业有限责任公司 | Preparation method of nano antimony pentoxide |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109988921A (en) * | 2019-04-17 | 2019-07-09 | 北京矿冶科技集团有限公司 | The method of antimony is separated in a kind of hydrochloric acid-chloride solution |
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