CN1108284C - Process for preparing barium carboxylate by reaction of witherite on carboxylic acid - Google Patents
Process for preparing barium carboxylate by reaction of witherite on carboxylic acid Download PDFInfo
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- CN1108284C CN1108284C CN00113761A CN00113761A CN1108284C CN 1108284 C CN1108284 C CN 1108284C CN 00113761 A CN00113761 A CN 00113761A CN 00113761 A CN00113761 A CN 00113761A CN 1108284 C CN1108284 C CN 1108284C
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- Prior art keywords
- carboxylic acid
- barium
- witherite
- acid barium
- reagent
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Abstract
The present invention relates to a preparation method of barium carboxylate, which is characterized in that natural witherite as a barium source instead of barium carbonate or barium hydroxide reacts with carboxylic acid, and the filter liquor is filtered to regulate the pH value of the filter liquor to be from 7 to 10; then, the filter liquor is heated, boiled and filtered once again to regulate the pH value of the filter liquor to be from 5 to 6.5; the filter liquor is evaporated and crystallized to obtain the barium carboxylate. The present invention has the advantages of short production flow, low product cost, stable product quality, low impurity content and no environmental pollution. The present invention is suitable for large-scale industrialized production.
Description
The preparation method who the present invention relates to carboxylic acid barium utilizes witherite and carboxylic acid effect to produce the novel method of carboxylic acid barium.
Current, many productions that formed plant-scale baric powder body material already both at home and abroad do not use carboxylic acid barium to be the barium source, but be the barium source with the barium carbonate, produce by solid reaction process, uneven, easily pollution that the various compositions of its composition of powder that this method makes disperse, particle diameter is thick and distribution range is wide, and the final material property of formation is not good.Carboxylic acid barium ((RCOO)
2Ba, R=H, CH
3, CH
3CH
2, CH
3CH
2CH
2) soluble in water, this character causes the concern of material supplier author to carboxylic acid barium already, the utilization homogeneous precipitation method, sol-gel method is the barium source with carboxylic acid barium, but powder body materials such as ferroelectric, the dielectric of industrial-scale production baric, piezoelectricity, pyroelectricity, superconduction, barium ferrite.Composition is even, granularity is ultra-fine and narrowly distributing because the powder body material that utilizes this technology to make has, and causes to form final excellent material performance.
; up at present; preparation SILVER REAGENT carboxylic acid barium still prolongs both at home and abroad with ancient traditional preparation method promptly uses SILVER REAGENT hydrated barta or SILVER REAGENT barium carbonate and SILVER REAGENT carboxylic acid (as acetate) effect to make (the elegant gold of " pure chemistry reagent " [Soviet Union] I-O.B. card; И. И. An Jieluofu work; Cao Suchen etc. translate; the Li Jiabin school, Higher Education Publishing House, 1989).The carboxylic acid barium cost height that this method makes.
The preparation method who the purpose of this invention is to provide a kind of carboxylic acid barium, overcome prior art system carboxylic acid barium cost height. the deficiency that price is expensive, produce cheap carboxylic acid barium reagent, for sol-gel method, the ultra-fine baric powder body material of homogeneous precipitation method industrial-scale production high-quality, to satisfy the growing needs of high performance material.
The object of the present invention is achieved like this:
The carboxylic acid effect of witherite or witherite powder and calculated amount is filtered, with saturated Ba (OH)
2Solution is regulated filtrate pH value to 7-10, heated and boiled then, filter once more, regulate filtrate pH value to 5-6.5 with corresponding carboxylic acid, being evaporated to crystallization separates out, cooling, filter, win time crystallization carboxylic acid barium, the crystallization that makes is dissolved in 2-4 water doubly and carries out recrystallization and can get secondary carboxylic acid barium reagent (press the detection of HGB3055-59 technological standard), seconds is carried out recrystallization again, make one-level carboxylic acid barium reagent (pressing the HGB3055-59 technological standard detects), the mother liquor of firsts and seconds product is merged evaporation, crystallization can make three grades of carboxylic acid barium reagent (pressing the HGB3055-59 technological standard detects), the mother liquor of three grades of product and the 1st subcrystalline mother liquor merge, evaporation, crystallization can make technical grade carboxylic acid barium (carboxylic acid barium content is greater than 90% after testing).The used carboxylic acid of the present invention is RCOOH (R=H, CH
3, CH
3CH
2, CH
3CH
2CH
2).If contain Fe in the witherite
2O
3, then add its iron ion mole number 0.5-1.0 30%H doubly in witherite and the carboxylic acid effect after-filtration gained filtrate
2O
2Solution is used saturated Ba (OH) then
2Solution transfers to 7-10 with pH value; If contain 10% above CaCO in the witherite
3, then in witherite and the carboxylic acid effect after-filtration gained filtrate, also must add 0.5-1.0 times of oxalic acid of its calcium ion mole number.
The used witherite raw material of the present invention originates from the Ankang Prefecture, and is as shown in table 1 from different ore deposit point sampling check and analysis results:
| Numbering | BaCO 3％ | CaCO 3％ | SiO 2％ | S％ | P％ | MgO％ | Al 2O 3％ | Fe 2O 3％ |
| 1 | 69.55 | 6.60 | 5.16 | 5.46 | -- | 3.69 | 0.26 | 0.86 |
| 2 | 44.59 | 10.12 | 20.63 | 3.38 | 0.065 | 1.80 | -- | -- |
| 3 | 63.06 | 3.25 | 1.84 | 0.02 | 0.07 | 0.13 | 0.27 | -- |
| 4 | 49.41 | 19.32 | 5.16 | 0.05 | 0.075 | 1.69 | 0.26 | 0.86 |
Table 1
Advantage of the present invention: a. adopts witherite and the effect of technical grade carboxylic acid, and Production Flow Chart is short, the rate of recovery height of barium, and product cost is low; B. utilize hydrogen peroxide and saturated oxalic acid liquid to make cleaner, make constant product quality, foreign matter content is little; C. the present invention is suitable for large-scale industrial production, and environmentally safe; D. the carboxylic acid barium produced of the present invention is except that can be used as reagent, also is suitable for being used for the barium source of superfine powdery material of the materials such as ferroelectric, dielectric, piezoelectricity, pyroelectricity, superconduction, barium ferrite of baric especially.
Directly producing carboxylic acid barium with witherite and carboxylic acid effect below is that example is described in detail implementation procedure of the present invention:
Embodiment 1:
In the 2000ml beaker, add 291 gram technical grade 50% aqueous formic acid and 700ml water, under agitation add witherite powder (table 1 numbering 2 breezes) 700 grams gradually till bubbling not, filter, in filtrate, add 50 gram oxalic acid, with saturated Ba (OH)
2Solution transfers to 7 with pH value, heated and boiled, and suction filtration transfers to 6.5 with 50% formic acid solution with filtrate pH value, evaporation, crystallisation by cooling, filtration, washing, drying get the 1st crystallization.The water that the 1st crystallization is dissolved in 2 times of weights carries out recrystallization, makes about 70 grams of secondary barium formate reagent; Seconds is carried out recrystallization again, can make about 14 grams of one-level barium formate reagent; With mother liquor merging, evaporation, the crystallization of firsts and seconds product, make three grades of about 38 grams of barium formate reagent again.Three grades of product mother liquors and the 1st subcrystalline mother liquor are merged, and evaporation, crystallization can make about 160 grams of technical grade barium formate.
Embodiment 2:
In the 3000ml beaker, add 278 gram technical grade butyric acid and 700ml water, under agitation add witherite powder (table 1 numbering 2 breezes) 700 grams gradually till bubbling not, filter, in filtrate, add 50 gram oxalic acid, with saturated Ba (OH)
2Solution transfers to 10 with pH value, heated and boiled, and suction filtration transfers to 6.0 with butyric acid solution with filtrate pH value, evaporation, crystallisation by cooling, filtration, washing, drying get the 1st crystallization.The water that the 1st crystallization is dissolved in 2 times of weights carries out recrystallization, makes about 95 grams of secondary butyric acid barium reagent; Seconds is carried out recrystallization again, can make about 19 grams of one-level butyric acid barium reagent; With mother liquor merging, evaporation, the crystallization of firsts and seconds product, make three grades of about 50 grams of butyric acid barium reagent again.Three grades of product mother liquors and the 1st subcrystalline mother liquor are merged, and evaporation, crystallization can make about 229 grams of technical grade butyric acid barium.
Embodiment 3:
In the 5000ml beaker, add 900 gram technical grade 50% aqueous formic acid and 2000ml water, under agitation add the witherite powder gradually, till bubbling not, added witherite powder (table 1 numbering 4 breezes) 2000 grams, there have slightly to be excessive, filter, add 20 milliliters of 30%H
2O
2With 260 gram oxalic acid, filtrate is with saturated Ba (OH)
2It is 9 that solution is regulated pH, heated and boiled, suction filtration, solution is regulated pH value to 6.5 with 50% aqueous formic acid, can make about 220 grams of secondary barium formate according to aforesaid method, and seconds is carried out recrystallization again, can make about 42 grams of one-level barium formate, mother liquor with the firsts and seconds product merges again, and evaporation, crystallization can make three grades of about 110 grams of barium formate.With three grades of product mother liquors and crystalline mother liquor merging for the first time, evaporation, crystallization can make technical grade barium formate 520 grams.
Embodiment 4:
According to aforesaid method, in the 3000ml beaker, add 410 gram technical grade Glacial acetic acid and 1600ml water, with 1000 gram witherite powder (table 1 numbering 1 breeze) reaction, filter, add 10 milliliters of 30%H
2O
2Solution is with Ba (OH)
2Solution transfers to 8 with filtrate pH, heated and boiled, and suction filtration transfers to 5.5 with Glacial acetic acid with the pH value of solution value, and through evaporation, crystallization, filtration, drying, time crystallization of winning is carried out recrystallization with crystallization for the first time, makes about 183 grams of secondary barium acetate reagent; Seconds is carried out recrystallization again, can make about 36 grams of one-level barium acetate reagent; With mother liquor merging, evaporation, the crystallization of firsts and seconds product, make three grades of about 95 grams of barium acetate reagent again.With three grades of product mother liquors and crystalline mother liquor merging for the first time, evaporation, crystallization can make about 450 grams of technical grade barium acetate.
Embodiment 5:
In 10 liters of beakers, add 750 gram technical grade acetate and 3000ml water, under agitation add witherite powder (table 1 numbering 3 breezes) 2000 grams gradually, filter, filtrate pH is with saturated Ba (OH)
2Solution transfers to 7.5, heated and boiled, and suction filtration, it is 6.5 that solution transfers to the pH value with Glacial acetic acid, evaporation, crystallisation by cooling, filtration, washing, drying get the 1st crystallization.Recrystallization is carried out in the 1st crystallization, make about 342 grams of secondary barium acetate reagent; Seconds is carried out recrystallization again, can make about 68 grams of one-level barium acetate reagent; With mother liquor merging, evaporation, the crystallization of firsts and seconds product, make three grades of about 170 grams of barium acetate reagent again.Three grades of product mother liquors and the 1st subcrystalline mother liquor are merged, and evaporation, crystallization can make about 750 grams of technical grade barium acetate.
Claims (7)
1. the method for carboxylic acid barium is produced in witherite and carboxylic acid effect, it is characterized in that: the carboxylic acid effect of witherite and calculated amount, by filter, with saturated Ba (OH)
2Solution is regulated filtrate pH value to 7-10, and heated and boiled is filtered once more then, regulates filtrate pH to 5-6.5 with corresponding carboxylic acid, and evaporative crystallization gets carboxylic acid barium, and used carboxylic acid is RCOOH, R=H, CH
3, CH
3CH
2Or CH
3CH
2CH
2
2. according to the described method for preparing carboxylic acid barium of claim 1, it is characterized in that adding in witherite and the carboxylic acid effect after-filtration gained filtrate 0.5-1.0 30%H doubly of its iron ion mole number
2O
2Solution, and with saturated Ba (OH)
2Solution transfers to 7-10 with pH value.
3. according to claim 1 or the 2 described methods that prepare carboxylic acid barium, it is characterized in that also having added in witherite and the carboxylic acid effect after-filtration gained filtrate 0.5-1.0 oxalic acid doubly of its calcium ion mole number, use saturated Ba (OH) then
2Solution transfers to 7-10 with pH value.
4. according to the described method for preparing carboxylic acid barium of claim 1, it is characterized in that the crystallization that makes is dissolved in 2-4 water doubly and carries out recrystallization and can get secondary carboxylic acid barium reagent.
5. according to the described method for preparing carboxylic acid barium of claim 4, it is characterized in that second class grade chemical is carried out recrystallization, can make one-level carboxylic acid barium reagent.
6. according to claim 4 or the 5 described methods that prepare carboxylic acid barium, it is characterized in that the mother liquor of one-level reagent and second class grade chemical is merged, evaporation, crystallization can make three grades of carboxylic acid barium reagent.
7. according to the described method for preparing carboxylic acid barium of claim 6, it is characterized in that evaporation, crystallization can make technical grade carboxylic acid barium with the mother liquor of three grades of reagent and crystalline mother liquor merging for the first time.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00113761A CN1108284C (en) | 2000-03-16 | 2000-03-16 | Process for preparing barium carboxylate by reaction of witherite on carboxylic acid |
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|---|---|---|---|
| CN00113761A CN1108284C (en) | 2000-03-16 | 2000-03-16 | Process for preparing barium carboxylate by reaction of witherite on carboxylic acid |
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|---|---|
| CN1271718A CN1271718A (en) | 2000-11-01 |
| CN1108284C true CN1108284C (en) | 2003-05-14 |
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|---|---|---|---|
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2792574C1 (en) * | 2022-06-29 | 2023-03-22 | Федеральное государственное автономное образовательное учреждение высшего образования "Пермский государственный национальный исследовательский университет" | Method for obtaining barium formate |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103360235A (en) * | 2013-08-14 | 2013-10-23 | 重庆新申世纪化工有限公司 | Preparation method of barium acetate |
| CN106565463A (en) * | 2016-11-22 | 2017-04-19 | 重庆新申世纪化工有限公司 | Preparation process of barium acetate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02215743A (en) * | 1989-02-15 | 1990-08-28 | Sannopuko Kk | Production of aqueous dispersion of carboxylic acid salt |
| WO1992006945A1 (en) * | 1990-10-19 | 1992-04-30 | Exxon Chemical Patents Inc. | Metal carboxylates |
-
2000
- 2000-03-16 CN CN00113761A patent/CN1108284C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02215743A (en) * | 1989-02-15 | 1990-08-28 | Sannopuko Kk | Production of aqueous dispersion of carboxylic acid salt |
| WO1992006945A1 (en) * | 1990-10-19 | 1992-04-30 | Exxon Chemical Patents Inc. | Metal carboxylates |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2792574C1 (en) * | 2022-06-29 | 2023-03-22 | Федеральное государственное автономное образовательное учреждение высшего образования "Пермский государственный национальный исследовательский университет" | Method for obtaining barium formate |
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| Publication number | Publication date |
|---|---|
| CN1271718A (en) | 2000-11-01 |
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