CN106115761A - A kind of method utilizing useless hydrobromic acid to prepare calcium bromide liquid - Google Patents
A kind of method utilizing useless hydrobromic acid to prepare calcium bromide liquid Download PDFInfo
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- CN106115761A CN106115761A CN201610481527.XA CN201610481527A CN106115761A CN 106115761 A CN106115761 A CN 106115761A CN 201610481527 A CN201610481527 A CN 201610481527A CN 106115761 A CN106115761 A CN 106115761A
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- mixed liquor
- hydrobromic acid
- useless
- calcium bromide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/20—Halides
- C01F11/34—Bromides
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Abstract
The present invention relates to a kind of method utilizing useless hydrobromic acid to prepare calcium bromide liquid, comprise the following steps: 1) quick lime is mixed with useless hydrobromic acid, and stir, prepare the first mixed liquor；2) again adding useless hydrobromic acid reaction in the first mixed liquor of step 1) gained, regulate PH, making reacted PH is 26, prepares the second mixed liquor；3) in the second mixed liquor, add reducing agent, prepare the 3rd mixed liquor；4) will add adsorbing medium in the 3rd mixed liquor of step 3) gained and heat, heating-up temperature is 70 130 DEG C, prepares the 4th mixed liquor；5) by the 4th mixed liquor regulation pH to 3 8.5, heat at temperature is 80 140 DEG C, the most concentrated, be filtrated to get solution of calcium bromide in water.There is production efficiency height, the feature of low cost compared with prior art.
Description
Technical field
The present invention relates to a kind of method preparing calcium bromide, specifically a kind of useless hydrobromic acid of utilization prepares calcium bromide liquid
The method of body.
Background technology
Calcium bromide is extensively applied in field of oil drilling, is mainly used as offshore oil drilling completion fluid, cementing fluid, well workover
Liquid, owing to can improve crude oil output capacity greatly, and receives significant attention.The preparation method of traditional calcium bromide is usually
With finished product bromine as raw material, production cost height is apparent from.
At present for reducing production cost, extensively with quick lime cheap and easy to get as raw material, react with hydrobromic acid and prepare bromine
Changing calcium solution, calcium bromide production technology is simplified by the method, and the production cost of calcium bromide can be made to be greatly lowered.But, due to
The usage amount of calcium bromide solution is very big, and Production requirement amount is relatively big, and hydrobromic cost still accounts for the biggest in actual production process
Ratio.In industry actual production, the useless hydrobromic acid amount of generation is the most more, but can not get well utilizing, and causes huge
Waste, if re-used by useless hydrobromic acid, can make the production cost of calcium bromide solution again reduce, and creates bigger for enterprise
Interests.Owing to useless hydrobromic acid existing the by-product acid of a lot of organic reaction, use the preparation method of existing calcium bromide solution, it is impossible to
Realize the removing of the impurity such as Organic substance in useless hydrobromic acid, have a strong impact on product final mass.
Summary of the invention
The present invention proposes a kind of method utilizing useless hydrobromic acid to prepare calcium bromide liquid.
The technical scheme is that and be achieved in that: a kind of method utilizing useless hydrobromic acid to prepare calcium bromide liquid, bag
Include following steps:
1) quick lime is mixed with useless hydrobromic acid, and stir, prepare the first mixed liquor；
2) again adding useless hydrobromic acid reaction in the first mixed liquor of step 1) gained, regulate PH, making reacted PH is 2-
6, prepare the second mixed liquor；Secondary adds useless hydrobromic acid to regulate solution to suitable PH, to facilitate the removing of impurity in solution；
3) in the second mixed liquor, add reducing agent, prepare the 3rd mixed liquor；
4) will add adsorbing medium heating in the 3rd mixed liquor of step 3) gained, heating-up temperature is 70-130 DEG C, prepares the
Four mixed liquors；At such a temperature, on the one hand will not affect impurity-eliminating effect because temperature is too low, on the other hand adsorbing medium can be made to protect
Hold optimal field of activity, impurity is had the strongest adsorption；
5) the 4th mixed liquor is added quick lime regulation pH to 3-8.5, heats at temperature is 80-140 DEG C, the most concentrated, mistake
Filter obtains solution of calcium bromide in water.
As preferred technical scheme, in step 1), quick lime and useless hydrobromic acid be that the ratio of 1:1 ~ 1:2 is mixed in mass ratio
Closing, stirring incorporation time is 0.5-1.5h.
As preferred technical scheme, step 2) in the first mixed liquor be 1:1-1:2 with useless hydrobromic mass ratio.
As preferred technical scheme, step 2) in the first mixed liquor be 30 ~ 80 DEG C with useless hydrobromic reaction temperature, instead
It is 3-5h between Ying Shi.
As preferred technical scheme, described reducing agent is carbamide, and consumption is the 1 ‰-3 ‰ of the second mixed liquor quality.
As preferred technical scheme, the purity of described quick lime is more than 95%, and described useless hydrobromic acid mass concentration is
40%-41%.
As preferred technical scheme, the addition of described adsorbing medium is the 0.5%-1% of the 3rd mixed liquor quality, institute
State adsorbing medium be in activated carbon, active hargil, kieselguhr, attapulgite any one or a few.
As preferred technical scheme, the heat time heating time in step 4) is 0.5-2h.
As preferred technical scheme, the heat time heating time in step 5) is 0.5-1.5h.
As preferred technical scheme, step 5) adds the 0.1%-that amount is the 4th mixed liquor quality of quick lime
0.5%.
Owing to have employed technique scheme, the present invention has a beneficial effect highlighted below:
1, the present invention utilizes Industry Waste hydrobromic acid to react with quick lime, produces calcium bromide solution, and in preparation process, regulation is suitable
Operating temperature, build suitable pH value working environment, the convenient impurity removing the more difficult separation such as Organic substance, coordinate absorption simultaneously
Medium adsorbs, and suitable operating temperature makes the field of activity that adsorbing medium holding is optimal, facilitates impurity to remove, with existing technique phase
Ratio, the present invention, without using refined hydrobromic acid or bromine to carry out calcium bromide production, saves great amount of cost, and it is steady to obtain quality
Fixed calcium bromide solution, preparation method efficiency is high.
2, good impurity removing effect, utilizes the calcium bromide solution that useless hydrobromic acid prepares, with the bromine prepared by refined hydrobromic acid
Change calcium solution to compare, the product quality indifference opposite sex of formation, form the product with grade, low cost, and useless hydrobromic acid is reclaimed
Utilize, environmental protection.
Detailed description of the invention
Technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that described enforcement
Example is only a part of embodiment of the present invention rather than whole embodiments.Based on the embodiment in the present invention, this area is common
The every other embodiment that technical staff is obtained under not making creative work premise, broadly falls into the model of present invention protection
Enclose.
Embodiment 1
A kind of method utilizing useless hydrobromic acid to prepare calcium bromide liquid, comprises the following steps:
1) quick lime that purity is 97% and the useless hydrobromic acid that mass concentration is 40% are mixed for the ratio of 1:1 in mass ratio,
And stir 0.5h to uniformly, prepare the first mixed liquor；
2) again add in the first mixed liquor of step 1) gained mass concentration be 40% give up hydrobromic acid reaction, be 30 in temperature
Reacting 5h under the conditions of DEG C, the first mixed liquor is 1:2 with useless hydrobromic mass ratio, regulates PH, and making reacted PH is 2, prepares
Second mixed liquor；
3) in the second mixed liquor, add the carbamide of the second mixed liquor quality 1 ‰, prepare the 3rd mixed liquor；
4) the 3rd mixed liquor of step 3) gained will add the activated carbon of the 3rd mixed liquor quality 0.5% and be heated to 70 DEG C,
Heating 2h, prepares the 4th mixed liquor；
5) will add the 0.5% of the 4th mixed liquor quality in the 4th mixed liquor, purity is the quick lime of 97%, regulates pH to 3, in temperature
Degree is to heat at 80 DEG C, heats 1.5h, the most concentrated, be filtrated to get solution of calcium bromide in water.
Embodiment 2
A kind of method utilizing useless hydrobromic acid to prepare calcium bromide liquid, comprises the following steps:
1) quick lime that purity is 97% and the useless hydrobromic acid that mass concentration is 41% are mixed for the ratio of 1:2 in mass ratio,
And stir 1.5h to uniformly, prepare the first mixed liquor；
2) again add in the first mixed liquor of step 1) gained mass concentration be 41% give up hydrobromic acid reaction, be 80 in temperature
Reacting 3h under the conditions of DEG C, the first mixed liquor is 1:1 with useless hydrobromic mass ratio, regulates PH, and making reacted PH is 6, prepares
Second mixed liquor；
3) in the second mixed liquor, add the carbamide of the second mixed liquor quality 3 ‰, prepare the 3rd mixed liquor；
4) the 3rd mixed liquor of step 3) gained will add the active hargil of the 3rd mixed liquor quality 1% and be heated to 130 DEG C,
Heating 0.5h, prepares the 4th mixed liquor；
5) will add the 0.1% of the 4th mixed liquor quality in the 4th mixed liquor, purity is the quick lime of 97%, regulates pH to 8.5,
Temperature is to heat at 140 DEG C, heats 0.5h, the most concentrated, be filtrated to get solution of calcium bromide in water.
Embodiment 3
A kind of method utilizing useless hydrobromic acid to prepare calcium bromide liquid, comprises the following steps:
1) quick lime that purity is 97% and the useless hydrobromic acid that mass concentration is 40% are mixed for the ratio of 1:1.5 in mass ratio
Close, and stir 1h to uniformly, prepare the first mixed liquor；
2) again add in the first mixed liquor of step 1) gained mass concentration be 40% give up hydrobromic acid reaction, be 55 in temperature
Reacting 4h under the conditions of DEG C, the first mixed liquor is 1:1.5 with useless hydrobromic mass ratio, regulates PH, and making reacted PH is 4, system
Obtain the second mixed liquor；
3) in the second mixed liquor, add the carbamide of the second mixed liquor quality 2 ‰, prepare the 3rd mixed liquor；
4) the 3rd mixed liquor of step 3) gained will add the kieselguhr of the 3rd mixed liquor quality 0.75% and be heated to 100
DEG C, heat 1h, prepare the 4th mixed liquor；
5) will add the 0.3% of the 4th mixed liquor quality in the 4th mixed liquor, purity is the quick lime of 97%, regulates pH to 5, in temperature
Degree is to heat at 110 DEG C, heats 1h, the most concentrated, be filtrated to get solution of calcium bromide in water.
Reference examples 1
A kind of method utilizing useless hydrobromic acid to prepare calcium bromide liquid, comprises the following steps:
1) quick lime that purity is 97% and the useless hydrobromic acid that mass concentration is 40% are mixed for the ratio of 1:1.5 in mass ratio
Close, and stir 1h to uniformly, prepare the first mixed liquor；
2) again add in the first mixed liquor of step 1) gained mass concentration be 40% give up hydrobromic acid reaction, be 55 in temperature
Reacting 4h under the conditions of DEG C, regulate PH, making reacted PH is 7, prepares the second mixed liquor；
3) in the second mixed liquor, add the carbamide of the second mixed liquor quality 2 ‰, prepare the 3rd mixed liquor；
4) the 3rd mixed liquor of step 3) gained will add the kieselguhr of the 3rd mixed liquor quality 0.75% and be heated to 100
DEG C, heat 1h, prepare the 4th mixed liquor；
5) by the 4th mixed liquor regulation pH to 5, heat at temperature is 110 DEG C, heat 1h, the most concentrated, be filtrated to get bromine
Change calcium aqueous solution.
Reference examples 2
A kind of method utilizing useless hydrobromic acid to prepare calcium bromide liquid, comprises the following steps:
1) quick lime that purity is 97% and the useless hydrobromic acid that mass concentration is 40% are mixed for the ratio of 1:1.5 in mass ratio
Close, and stir 1h to uniformly, prepare the first mixed liquor；
2) again add in the first mixed liquor of step 1) gained mass concentration be 40% give up hydrobromic acid reaction, be 55 in temperature
Reacting 4h under the conditions of DEG C, the first mixed liquor is 1:1.5 with useless hydrobromic mass ratio, regulates PH, and making reacted PH is 4, system
Obtain the second mixed liquor；
3) in the second mixed liquor, add the carbamide of the second mixed liquor quality 2 ‰, prepare the 3rd mixed liquor；
4) the 3rd mixed liquor of step 3) gained will add the kieselguhr of the 3rd mixed liquor quality 0.75% and be heated to 135
DEG C, heat 1h, prepare the 4th mixed liquor；
5) will add the 0.3% of the 4th mixed liquor quality in the 4th mixed liquor, purity is the quick lime of 97%, regulates pH to 5, in temperature
Degree is to heat at 110 DEG C, heats 1h, the most concentrated, be filtrated to get solution of calcium bromide in water.
Reference examples 3
A kind of method utilizing useless hydrobromic acid to prepare calcium bromide liquid, comprises the following steps:
1) quick lime that purity is 97% and the useless hydrobromic acid that mass concentration is 40% are mixed for the ratio of 1:1.5 in mass ratio
Close, and stir 1h to uniformly, prepare the first mixed liquor；
2) again add in the first mixed liquor of step 1) gained mass concentration be 40% give up hydrobromic acid reaction, be 55 in temperature
Reacting 4h under the conditions of DEG C, the first mixed liquor is 1:1.5 with useless hydrobromic mass ratio, regulates PH, and making reacted PH is 4, system
Obtain the second mixed liquor；
3) in the second mixed liquor, add the carbamide of the second mixed liquor quality 2 ‰, prepare the 3rd mixed liquor；
4) the 3rd mixed liquor of step 3) gained will add the kieselguhr of the 3rd mixed liquor quality 0.75% and be heated to 100
DEG C, heat 1h, prepare the 4th mixed liquor；
5) the 4th mixed liquor will add the quick lime that purity is 97%, regulate pH to 9, heat at temperature is 110 DEG C, heating
1h, the most concentrated, be filtrated to get solution of calcium bromide in water.
Being chemically examined by the calcium bromide product of the embodiment of the present invention and reference examples gained, result is as shown in the table.
As seen from the above table, the product quality prepared by embodiment of the present invention 1-3 meets required standard, and reference examples 1-3 change side
Temperature parameter in method, PH parameter, all can produce impact to this product quality.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention
Within god and principle, any modification, equivalent substitution and improvement etc. made, should be included within the scope of the present invention.
Claims (10)
1. one kind utilizes the method that useless hydrobromic acid prepares calcium bromide liquid, it is characterised in that comprise the following steps:
1) quick lime is mixed with useless hydrobromic acid, and stir, prepare the first mixed liquor；
2) in step 1) the first mixed liquor of gained adds useless hydrobromic acid reaction again, regulate PH, making reacted PH is 2-
6, prepare the second mixed liquor；
3) in the second mixed liquor, add reducing agent, prepare the 3rd mixed liquor；
4) by step 3) the 3rd mixed liquor of gained adds adsorbing medium and heats, heating-up temperature is 70-130 DEG C, prepares the
Four mixed liquors；
5) the 4th mixed liquor is added quick lime regulation pH to 3-8.5, heats at temperature is 80-140 DEG C, the most concentrated, mistake
Filter obtains solution of calcium bromide in water.
2. according to a kind of method utilizing useless hydrobromic acid to prepare calcium bromide liquid described in claim 1, it is characterised in that: step
1) in, quick lime and useless hydrobromic acid ratio for 1:1-1:2 in mass ratio mixes, and stirring incorporation time is 0.5-1.5h.
3. according to a kind of method utilizing useless hydrobromic acid to prepare calcium bromide liquid described in claim 1, it is characterised in that: step
2) in, the first mixed liquor is 1:1-1:2 with useless hydrobromic mass ratio.
4. according to a kind of method utilizing useless hydrobromic acid to prepare calcium bromide liquid described in claim 1, it is characterised in that: step
2) in, the first mixed liquor is 30～80 DEG C with useless hydrobromic reaction temperature, and the response time is 3-5h.
5. according to a kind of method utilizing useless hydrobromic acid to prepare calcium bromide liquid described in claim 1, it is characterised in that: described
Reducing agent be carbamide, consumption is the 1 ‰-3 ‰ of the second mixed liquor quality.
6. according to a kind of method utilizing useless hydrobromic acid to prepare calcium bromide liquid described in claim 1, it is characterised in that: described
The purity of quick lime is more than 95%, and described useless hydrobromic acid mass concentration is 40%-41%.
7. according to a kind of method utilizing useless hydrobromic acid to prepare calcium bromide liquid described in claim 1, it is characterised in that: described
The addition of adsorbing medium is the 0.5%-1% of the 3rd mixed liquor quality, and described adsorbing medium is activated carbon, active hargil, silicon
In diatomaceous earth, attapulgite any one or a few.
8. according to a kind of method utilizing useless hydrobromic acid to prepare calcium bromide liquid described in claim 1, it is characterised in that: step
4) heat time heating time in is 0.5-2h.
9. according to a kind of method utilizing useless hydrobromic acid to prepare calcium bromide liquid described in claim 1, it is characterised in that: step
5) heat time heating time in is 0.5-1.5h.
10. according to a kind of method utilizing useless hydrobromic acid to prepare calcium bromide liquid described in claim 1, it is characterised in that: step
Rapid 5) 0.1%-0.5% that amount is the 4th mixed liquor quality of quick lime is added in.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4234556A (en) * | 1979-10-05 | 1980-11-18 | The Dow Chemical Company | Method of producing calcium bromide |
| EP1585706A1 (en) * | 2002-12-02 | 2005-10-19 | Bromine Compounds Ltd. | Process for the preparation of cabr2 hydrates and uses thereof |
| CN101391748A (en) * | 2008-10-29 | 2009-03-25 | 袁景海 | Method for preparing oilfield additive calcium bromide |
| CN101618888A (en) * | 2009-08-03 | 2010-01-06 | 山东天信化工有限公司 | Method for preparing calcium bromide solution used for oil drilling |
-
2016
- 2016-06-26 CN CN201610481527.XA patent/CN106115761A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4234556A (en) * | 1979-10-05 | 1980-11-18 | The Dow Chemical Company | Method of producing calcium bromide |
| EP1585706A1 (en) * | 2002-12-02 | 2005-10-19 | Bromine Compounds Ltd. | Process for the preparation of cabr2 hydrates and uses thereof |
| CN101391748A (en) * | 2008-10-29 | 2009-03-25 | 袁景海 | Method for preparing oilfield additive calcium bromide |
| CN101618888A (en) * | 2009-08-03 | 2010-01-06 | 山东天信化工有限公司 | Method for preparing calcium bromide solution used for oil drilling |
Non-Patent Citations (2)
| Title |
|---|
| 中国食品添加剂和配料协会: "《食品添加剂手册（第三版）》", 30 September 2012, 中国轻工业出版社 * |
| 孙建梅等: "新法制备溴化钙", 《天津化工》 * |
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Application publication date: 20161116 |