CN104402015A - Preparation method of high purity boric acid - Google Patents
Preparation method of high purity boric acid Download PDFInfo
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- CN104402015A CN104402015A CN201410603563.XA CN201410603563A CN104402015A CN 104402015 A CN104402015 A CN 104402015A CN 201410603563 A CN201410603563 A CN 201410603563A CN 104402015 A CN104402015 A CN 104402015A
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- boric acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
- C01B35/10—Compounds containing boron and oxygen
- C01B35/1045—Oxyacids
- C01B35/1054—Orthoboric acid
- C01B35/1063—Preparation from boron ores or borates using acids or salts
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Abstract
The invention relates to a preparation method of high purity boric acid. The preparation method comprises the following steps of accurately weighing a certain amount of analytically pure borax, putting the analytically pure borax into deionized water, carrying out magnetic stirring heating until complete dissolution, keeping a filtrate temperature, carrying out fast filtration by a quartz sand funnel, heating the filtrate by a constant-temperature water bath, feeding HCl gas into the filtrate to cause a borax neutralization reaction in a self-made kipp's generator, wherein in the reaction, a temperature is controlled, then detecting acidity pH of the solution, cooling the reaction product by a plurality of cooling methods, putting the cooled reaction product into a low-temperature constant-temperature tank at last, carrying out constant-temperature cooling crystallization, then carrying out centrifugation, carrying out vacuum suction filtration, carrying out washing, detecting a pH value of the surfaces of the crystals by a precision pH test paper, putting the crystals into a vacuum drying box, carrying out drying to obtain a boric acid crude product, and returning a mother liquor containing a less amount of boric acid and a sodium salt to acidolysis and neutralization processes for recycle. The preparation method adopts the raw materials with low prices, produces less by-products, has low energy consumption and can prepare high-purity boric acid easily.
Description
Technical field
The present invention relates to a kind of boric acid preparation method, particularly relate to a kind of high-purity boric acid preparation method.
Background technology
Boric acid is a kind of multi-functional industrial chemicals, occupies an important position in national economy and industrial and agricultural production development.Due to the restriction of conventional preparation techniques and low-grade boron resource, high-purity boracic acid not easily obtains at home, depends on import.In recent years, a large amount of import high-purity boracic acids enters China market, and compared with home products, external boric acid indices is all far away higher than the similar index of home products.High-purity boracic acid is used as high purity reagent and produces various high purity boron hydrochlorate crystal raw material, applies wider in high-tech area.
Therefore, it is high to seek a kind of synthesis purity, and material price preparation method that is cheap, that be convenient to large-scale commercial production is the key overcome the above problems.
Summary of the invention
Technical problem to be solved by this invention is to provide that a kind of method prices of raw and semifnished materials are cheap, by product is few, energy consumption is low, easily obtain the preparation method of high-purity boric acid.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of high-purity boric acid preparation method, comprises the steps:
Accurately take a certain amount of analytical pure borax in deionized water, magnetic agitation heats, and after dissolving completely, keeps filtrate temperature, with quartz sand funnel fast filtering;
Utilize water bath with thermostatic control to heat filtrate, adopt self-control kipp gas generator, pass in HCI gas and borax reaction, control temperature, after reaction, detect solution acidity pH;
Completely reacted material is chosen multiple cooling method, finally puts into low temperature thermostat bath, after constant temperature crystallisation by cooling, centrifugation, vacuum suction filter, washing, detects xln surface p H with accurate pH test paper;
Xln is placed in after vacuum drying oven is dried and namely obtains crude boronic acid, containing a small amount of boric acid and sodium salt in mother liquor, return in acidolysis and operation, recycle.
On the basis of technique scheme, the present invention can also do following improvement.
Further, describedly accurately take a certain amount of analytical pure borax in deionized water, magnetic agitation heats, and after dissolving completely, keeps filtrate temperature, with being implemented as follows of quartz sand funnel fast filtering step:
Accurately take a certain amount of analytical pure borax in deionized water, magnetic agitation is heated to 95 DEG C, after dissolving completely, keeps filtrate temperature at about 85 DEG C, with quartz sand funnel fast filtering.
Further, describedly utilize water bath with thermostatic control to heat filtrate, adopt self-control kipp gas generator, pass in HCI gas and borax reaction, control temperature, after reaction, detect being implemented as follows of solution acidity pH step:
Utilize water bath with thermostatic control to be heated to 90 DEG C to filtrate, adopt self-control kipp gas generator, pass in HCI gas and borax reaction, control temperature is no more than 102 DEG C, and after reaction 3 ~ 5min, detecting solution acidity pH is 3 ~ 4.
Further, multiple cooling method chosen by described just completely reacted material, finally puts into low temperature thermostat bath, after constant temperature crystallisation by cooling, and centrifugation, vacuum suction filter, washing, detects being implemented as follows of xln surface p H step with accurate pH test paper:
Completely reacted material is chosen multiple cooling method, finally puts into 8 DEG C of low temperature thermostat baths, after constant temperature crystallisation by cooling 8h, centrifugation, vacuum suction filter, washing, detecting xln surface p H with accurate pH test paper is 3 ~ 4.
Further, namely described being placed in by xln after vacuum drying oven is dried obtain crude boronic acid, containing a small amount of boric acid and sodium salt in mother liquor, returns in acidolysis and operation, being implemented as follows of recycle step:
Xln is placed in after 50 DEG C of vacuum drying ovens are dried and namely obtains crude boronic acid, containing a small amount of boric acid and sodium salt in mother liquor, return in acidolysis and operation, recycle.
The invention has the beneficial effects as follows: the method prices of raw and semifnished materials are cheap, by product is few, energy consumption is low, easily obtain high-purity boric acid.
Embodiment
Be described principle of the present invention and feature below in conjunction with embodiment, example, only for explaining the present invention, is not intended to limit scope of the present invention.
A kind of high-purity boric acid preparation method, comprises the steps:
Accurately take a certain amount of analytical pure borax in deionized water, magnetic agitation heats, and after dissolving completely, keeps filtrate temperature, with quartz sand funnel fast filtering;
Utilize water bath with thermostatic control to heat filtrate, adopt self-control kipp gas generator, pass in HCI gas and borax reaction, control temperature, after reaction, detect solution acidity pH;
Completely reacted material is chosen multiple cooling method, finally puts into low temperature thermostat bath, after constant temperature crystallisation by cooling, centrifugation, vacuum suction filter, washing, detects xln surface p H with accurate pH test paper;
Xln is placed in after vacuum drying oven is dried and namely obtains crude boronic acid, containing a small amount of boric acid and sodium salt in mother liquor, return in acidolysis and operation, recycle.
Embodiment 1:
Accurately take a certain amount of analytical pure borax in deionized water, magnetic agitation is heated to 95 DEG C, after dissolving completely, keeps filtrate temperature at about 85 DEG C, with quartz sand funnel fast filtering; Utilize water bath with thermostatic control to be heated to 90 DEG C to filtrate, adopt self-control kipp gas generator, pass in HCI gas and borax reaction, control temperature is no more than 102 DEG C, and after reaction 3min, detecting solution acidity pH is 3; Completely reacted material is chosen multiple cooling method, finally puts into 8 DEG C of low temperature thermostat baths, after constant temperature crystallisation by cooling 8h, centrifugation, vacuum suction filter, washing, detecting xln surface p H with accurate pH test paper is 3; Xln is placed in after 50 DEG C of vacuum drying ovens are dried and namely obtains crude boronic acid, containing a small amount of boric acid and sodium salt in mother liquor, return in acidolysis and operation, recycle.
Embodiment 2:
Accurately take a certain amount of analytical pure borax in deionized water, magnetic agitation is heated to 95 DEG C, after dissolving completely, keeps filtrate temperature at about 85 DEG C, with quartz sand funnel fast filtering; Utilize water bath with thermostatic control to be heated to 90 DEG C to filtrate, adopt self-control kipp gas generator, pass in HCI gas and borax reaction, control temperature is no more than 102 DEG C, and after reaction 4min, detecting solution acidity pH is 3.5; Completely reacted material is chosen multiple cooling method, finally puts into 8 DEG C of low temperature thermostat baths, after constant temperature crystallisation by cooling 8h, centrifugation, vacuum suction filter, washing, detecting xln surface p H with accurate pH test paper is 3.5; Xln is placed in after 50 DEG C of vacuum drying ovens are dried and namely obtains crude boronic acid, containing a small amount of boric acid and sodium salt in mother liquor, return in acidolysis and operation, recycle.
Embodiment 3:
Accurately take a certain amount of analytical pure borax in deionized water, magnetic agitation is heated to 95 DEG C, after dissolving completely, keeps filtrate temperature at about 85 DEG C, with quartz sand funnel fast filtering; Utilize water bath with thermostatic control to be heated to 90 DEG C to filtrate, adopt self-control kipp gas generator, pass in HCI gas and borax reaction, control temperature is no more than 102 DEG C, and after reaction 5min, detecting solution acidity pH is 4; Completely reacted material is chosen multiple cooling method, finally puts into 8 DEG C of low temperature thermostat baths, after constant temperature crystallisation by cooling 8h, centrifugation, vacuum suction filter, washing, detecting xln surface p H with accurate pH test paper is 4; Xln is placed in after 50 DEG C of vacuum drying ovens are dried and namely obtains crude boronic acid, containing a small amount of boric acid and sodium salt in mother liquor, return in acidolysis and operation, recycle.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. a high-purity boric acid preparation method, is characterized in that, comprises the steps:
Accurately take a certain amount of analytical pure borax in deionized water, magnetic agitation heats, and after dissolving completely, keeps filtrate temperature, with quartz sand funnel fast filtering;
Utilize water bath with thermostatic control to heat filtrate, adopt self-control kipp gas generator, pass in HCI gas and borax reaction, control temperature, after reaction, detect solution acidity pH;
Completely reacted material is chosen multiple cooling method, finally puts into low temperature thermostat bath, after constant temperature crystallisation by cooling, centrifugation, vacuum suction filter, washing, detects xln surface p H with accurate pH test paper;
Xln is placed in after vacuum drying oven is dried and namely obtains crude boronic acid, containing a small amount of boric acid and sodium salt in mother liquor, return in acidolysis and operation, recycle.
2. a kind of high-purity boric acid preparation method according to claim 1, is characterized in that, describedly accurately takes a certain amount of analytical pure borax in deionized water, magnetic agitation heats, after dissolving completely, keep filtrate temperature, with being implemented as follows of quartz sand funnel fast filtering step:
Accurately take a certain amount of analytical pure borax in deionized water, magnetic agitation is heated to 95 DEG C, after dissolving completely, keeps filtrate temperature at about 85 DEG C, with quartz sand funnel fast filtering.
3. a kind of high-purity boric acid preparation method according to claim 1, is characterized in that, describedly utilizes water bath with thermostatic control to heat filtrate, adopt self-control kipp gas generator, pass in HCI gas and borax reaction, control temperature, after reaction, detect being implemented as follows of solution acidity pH step:
Utilize water bath with thermostatic control to be heated to 90 DEG C to filtrate, adopt self-control kipp gas generator, pass in HCI gas and borax reaction, control temperature is no more than 102 DEG C, and after reaction 3 ~ 5 min, detecting solution acidity pH is 3 ~ 4.
4. a kind of high-purity boric acid preparation method according to claim 1, it is characterized in that, multiple cooling method chosen by described just completely reacted material, finally put into low temperature thermostat bath, after constant temperature crystallisation by cooling, centrifugation, vacuum suction filter, washing, detects being implemented as follows of xln surface p H step with accurate pH test paper:
Completely reacted material is chosen multiple cooling method, finally puts into 8 DEG C of low temperature thermostat baths, after constant temperature crystallisation by cooling 8 h, centrifugation, vacuum suction filter, washing, detecting xln surface p H with accurate pH test paper is 3 ~ 4.
5. a kind of high-purity boric acid preparation method according to claim 1, it is characterized in that, namely described being placed in by xln after vacuum drying oven is dried obtain crude boronic acid, containing a small amount of boric acid and sodium salt in mother liquor, return in acidolysis and operation, being implemented as follows of recycle step:
Xln is placed in after 50 DEG C of vacuum drying ovens are dried and namely obtains crude boronic acid, containing a small amount of boric acid and sodium salt in mother liquor, return in acidolysis and operation, recycle.
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|---|---|---|---|
| CN201410603563.XA CN104402015A (en) | 2014-10-31 | 2014-10-31 | Preparation method of high purity boric acid |
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| CN201410603563.XA CN104402015A (en) | 2014-10-31 | 2014-10-31 | Preparation method of high purity boric acid |
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| CN104402015A true CN104402015A (en) | 2015-03-11 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105347353A (en) * | 2015-12-17 | 2016-02-24 | 丹东市化学试剂厂 | Preparation method of high-purity boric acid |
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- 2014-10-31 CN CN201410603563.XA patent/CN104402015A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105347353A (en) * | 2015-12-17 | 2016-02-24 | 丹东市化学试剂厂 | Preparation method of high-purity boric acid |
| CN105347353B (en) * | 2015-12-17 | 2017-10-13 | 丹东市化学试剂厂 | High-purity boracic acid preparation method |
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Application publication date: 20150311 |