CN101948118B - Preparation method of nuclear boric acid - Google Patents
Preparation method of nuclear boric acid Download PDFInfo
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- CN101948118B CN101948118B CN2010105007846A CN201010500784A CN101948118B CN 101948118 B CN101948118 B CN 101948118B CN 2010105007846 A CN2010105007846 A CN 2010105007846A CN 201010500784 A CN201010500784 A CN 201010500784A CN 101948118 B CN101948118 B CN 101948118B
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Abstract
The invention relates to a preparation method of a nuclear boric acid, which has the following characteristics of (1) using industrial boric acid, the H3BO3 mass percentage of which is 99%, as a raw material; (2) preparing nuclear boric acid with H3BO3 content not less than 99.95% by using a physical refining and purification method; and (3) in the process of physical refining and purification, enabling 30% of filtered slurry obtained after filtering to enteri a mother liquor through a loop for applying, mixing together with the added raw material and repeatedly applying 10-12 times for improving the yield. The product prepared by using the preparation method meets clean production and environmental friendliness; the raw material, the auxiliary material and ionized water are decreased by above 30%; and the energy consumption (electricity, coal and the like) is reduced. The product is physically refined and purified without waste gas, waste water and waste residues; the process flow is the key for the developed novel product; applying is repeatedly performed 10-12 times; the product is sampled and tested many times by Beijing Research Institute of Chemical Metallurgy, Ministry of Nuclear Industry, and the result is that all parameters (15 items), the content and the isotopes all exceed the specified technical targets of the nuclear power stations.
Description
Technical field
The present invention relates to a kind of preparation method who examines grade boric acid, belong to the stupalith field that Nuclear power plants uses.
Background technology
Boric acid is a kind of multi-functional important inorganic chemical industry basic raw material, in national economy and industrial production development, occupies an important position.High-purity boric acid is as high purity reagent and produce various high purity boron hydrochlorate crystalline raw materials, is that high-tech area is used wider industrial chemicals.In nuclear industry, the conduct of boron-10 isotropic substance is the thermal neutron absorption agent efficiently, is requisite in safety and the system.Particular stage (SQ) boric acid is used for nuclear industry, can partly replace isotropic substance boron-10.
For general pressurized water reactor, consider the cost problem, mostly use nuclear level sassolite as neutron moderator, trapping agent and refrigerant, and consumption is very big, the purity and the impurity index request of nuclear level boric acid are high.Although the working method of existing domestic and international boric acid has nothing in common with each other according to the difference of boron resource; But generally speaking; Still be main with acid system, the country from producing boric acid in the world at present mainly contains states such as the U.S., Turkey, Russia, Italy, Japan, China.Wherein leading with the U.S..It is reported (Zheng Xuejia; " Liaoning chemical industry " 2000 (5) PP276-278) U.S. borax chemical company is raw material with the tincal; Produce boric acid through sulfuric acid process, use the steam distillation method, under hot conditions more than 500 ℃, the boric acid in the acidolysis filtered liq is distilled; And for example osmanli Eti Holdlmg As company report is developed a kind of method through wet-chemical prepares boric acid from borax soln technology; The boric acid purity of utilizing this prepared is greater than 99.6% (A.Mergen et.al; Advanced powder Technology.14 (3), 2003).
Domestic research and development about the boric acid product start to walk a little later, but development in recent years rapidly, and are progressive very big.For example Ministry of Chemical Industry Changsha design and research institute researches and develops a kind of technology (CN1962440) of producing boric acid with the warwickite acid system; What and for example Nanjing JinMei Gallium Ltd. released is raw material with the guaranteed reagent, adopts IX and recrystallization bonded method to prepare purity and is higher than high-purity boric acid (CN101412519) of 99.5%.
In view of adding nuclear level boric acid in pressurized-water reactor-circuit cools agent is the indispensable subsidiary material that conditioned reaction heap safety is carried out; From above analysis to existing background technology; So far produce nuclear level boric acid both at home and abroad and all adopt the s.t. method; Even CN101412519 is a raw material with high-quality pure reagent, the method for purification and the designated products that adopt chemistry to combine with physics only are " high-purity boric acid " not mentioned " can be used for nuclear reactor ".
In view of above analysis, the present invention intends a kind of employing content 99% industrial boric acid is provided is raw material, produces the preparation method of content >=99.96% nuclear level boric acid with the refining method of purifying of physics.
Summary of the invention
The object of the present invention is to provide a kind of preparation method who examines grade boric acid.The invention is characterized in:
(i) with purity be the H of 99% (quality)
3BO
3Industrial boric acid be raw material;
(ii) prepare H with the refining method of purifying of physics
3BO
3The nuclear level boric acid of content>=99.95%;
(iii) in the refining preparation process of purifying of physics, filter slip with getting rid of 30% after the filter, get into mother liquid recycle through the loop, stir and repeat to apply mechanically 10-12 time with dropping into raw material again, thereby can improve the benefit rate more than 97%.
Specifically, preparation technology's flow process of nuclear level boric acid provided by the invention is as shown in Figure 1, the technical process of recycled:
(1) industrial boric acid with 99% (content) is a raw material;
(2) add the electronic-grade ionized water of million grades of a certain proportion of 5-8, the mass ratio of electronic-grade ionized water and industrial boric acid be (5-6): 1, and best the ratio is (5.0-5.2): 1;
(3) solution of step 2 being prepared carries out heated and stirred and becomes suspension-s, the about 0.5-2 of churning time hour (specifically deciding) according to dissolution degree, temperature about 80-90 ℃ with rotating speed 60-80 time/minute.
(4) carry out centrifuging through step 3 through the suspension-s that stirs, filtration temperature is 80-90 ℃;
(5) filtered liq after the filtration cools off recrystallization and dewatering and filtering; Cooling temperature is lower than 40 ℃, about 2-3 hour, decides according to crystallization degree.
(6) filter is got rid of in the electronic-grade ionized water rinsing that adds million grades of 5-8 more then, and the temperature of getting rid of filter is 30-40 ℃;
(7) get in the input raw material that the slurry that gets rid of filter back material 30% (volume) is back to step 2 preparation and carry out mother liquid recycle, repeat above-mentioned steps 2-7, repeat to apply mechanically 10-12 time;
(8) 70% entering that step 7 is stayed mixes subsider, the dry acquisition;
According to the prepared nuclear level boric acid of method provided by the invention through the Beijing Inst. of Chemical Metallurgy, Ministry of Nuclear Industry Institute of Analysis detect as shown in table 1, H
3BO
3Content is>=99.95-99.96%,
10B content is 19.80-19.92.
Table 1 detected result gathers
The product that is provided by working method of the present invention meets cleaner production and friendly environment, reduces raw and auxiliary material, ionized water, energy efficient (electric coal etc.) more than 30%.Product is because the refining purification of physics; The product innovation technical process of the no three wastes, exploitation is crucial; Carry out 10-12 time and apply mechanically repeatedly, product is tested through the multiple sampling of Beijing chemical metallurgy research institute of Ministry of Nuclear Industry: the technical indicator (seeing table 1) that parameters (15), content and isotropic substance are all stipulated above Nuclear power plants.
Description of drawings
Fig. 1 is preparing method's technical process provided by the invention.
Embodiment
Through the description of specific embodiment, further set forth substantive distinguishing features of the present invention and obvious improvement below.
Embodiment 1
A) with purity be the H of 99% (quality)
3BO
3Industrial boric acid is a raw material;
B) add the electronic-grade ionized water of million grades of a certain proportion of 5-8, the mass ratio of electronic-grade ionized water and industrial boric acid is 5.2: 1;
C) the solution heated and stirred with step b preparation becomes suspension-s, and wherein whipping temp is 80-90 ℃, and the time is 1 hour, and stirring velocity is 70 commentaries on classics/min;
D) suspension-s through step c carries out centrifuging, and filtration temperature is 80-85 ℃;
E) filtered liq after the filtration cools off recrystallization and dewatering and filtering; Cooling temperature is lower than 40 ℃, and the recrystallization time is 2.5 hours;
F) get rid of filter then after adding the electronic-grade ionized water rinsing of million grades of 5-8 again, the temperature of getting rid of filter is 30-35 ℃;
G) get the slip liquid backflow repeating step b that gets rid of filter back 30% (volume) and carry out mother liquid recycle, so repeat above-mentioned steps b)～g) 12 times;
H) 70% slurries that step g) stayed get into mixing subsider drying and obtain a nuclear level boric acid, and gained is examined the main rerum natura of level boric acid shown in (I) in the table 1, H
3BO
3Content is up to 99.96%,
10B is 19.80.
Embodiment 2
The mass ratio of electronic-grade ionized water and industrial boric acid is 5.5-1 among the step b, and all the other are with embodiment 1, and prepared nuclear level boric acid content is 99.95%,
10B is 19.92% (II in the table 1).
Embodiment 3
The mass ratio of electronic-grade ionized water and industrial boric acid is 6: 1 among the step b, and the filtration temperature of steps d is 85-90 ℃, and all the other are with embodiment 1, and prepared nuclear level boric acid content is 99.96%,
10B is 19.88% (III in the table 1).
Electronic-grade ionized water model used in the present invention is HRO-1020 first-stage reverse osmosis+EDI water treatment; Flow is 2T/H; By electric nuclear industry the 8th nuclear research institute, Yiming Filtering Technology Co., Ltd., Shanghai and nuclear industry purification filtering engineering center cooperative research and development, it is 5M Ω CM that system produces the water resistance rate.
Claims (7)
1. preparation method who examines grade boric acid is characterized in that:
(i) be that 99% industrial boric acid is a raw material with mass percent;
(ii) prepare H with the refining method of purifying of physics
3BO
3The nuclear level boric acid of content>=99.95%;
(iii) in the refining preparation process of purifying of physics, filter slip with getting rid of 30% after the filter, get into mother liquid recycle through the loop, stir and repeat to apply mechanically 10-12 time with dropping into raw material again, thereby with raising benefit rate;
Concrete process step is:
(1) be that 99% industrial boric acid is a raw material with mass percent;
(2) add the electronic-grade ionized water of million grades of a certain proportion of 5-8, the mass ratio of described electronic-grade ionized water and industrial boric acid is (5-6): 1;
(3) solution of step (2) being prepared carries out heated and stirred and becomes suspension-s, and churning time is 0.5-2 hour, and temperature is controlled at 80-90 ℃;
(4) carry out centrifuging through step (3) through the suspension-s that stirs, filtration temperature is 80-90 ℃;
(5) filtered liq after the filtration cools off recrystallization and dewatering and filtering; Cooling temperature is lower than 40 ℃;
(6) filter is got rid of in the electronic-grade ionized water rinsing that adds million grades of 5-8 more then, and the temperature of getting rid of filter is 30-40 ℃;
(7) get that to get rid of filter back percent by volume be that 30% slip joins in the input raw material of step (2) preparation and carries out mother liquid recycle, repeat above-mentioned steps (2)-(7), repeat to apply mechanically 10-12 time;
(8) 70% the slip that step (7) is stayed gets into and mixes subsider, the dry nuclear level boric acid that obtains.
2. by the described method of claim 1, it is characterized in that the mass ratio of electronic-grade ionized water described in the step (2) and industrial boric acid is (5.0-5.2): 1.
3. by the described method of claim 1, the rotating speed when it is characterized in that stirring in the step (3) is 60-80 time/minute.
4. by the described method of claim 2, it is characterized in that in the step (3):
Churning time is 1 hour; Rotating speed during stirring is 70 rev/mins.
5. by the described method of claim 1, it is characterized in that the described cooling temperature of step (5) is lower than 40 ℃, the recrystallization time is 2-3 hour.
6. by the described method of claim 1, it is characterized in that the electronic-grade ionized water resistivity described in step (2) and the step (6) is 5M Ω cm.
7. by the described method of claim 1, it is characterized in that mother liquor repeats to apply mechanically 12 times.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010105007846A CN101948118B (en) | 2010-09-30 | 2010-09-30 | Preparation method of nuclear boric acid |
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| CN2010105007846A CN101948118B (en) | 2010-09-30 | 2010-09-30 | Preparation method of nuclear boric acid |
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| CN101948118A CN101948118A (en) | 2011-01-19 |
| CN101948118B true CN101948118B (en) | 2012-02-01 |
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| CN2010105007846A Active CN101948118B (en) | 2010-09-30 | 2010-09-30 | Preparation method of nuclear boric acid |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104045094B (en) * | 2013-11-13 | 2018-04-03 | 中广核工程有限公司 | Boron device processed and boron method processed for nuclear power station |
| CN110054196B (en) * | 2019-04-10 | 2022-04-15 | 大连理工大学 | Method for preparing high-purity spherical instant boric acid by organic molecule induction |
| CN110255577B (en) * | 2019-06-05 | 2021-10-22 | 核工业北京化工冶金研究院 | Preparation process of nuclear pure grade boric acid standard substance |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1484860A (en) * | 1973-11-22 | 1977-09-08 | United States Borax Chem | Manufacture of boric acid |
| JPH01119511A (en) * | 1987-10-30 | 1989-05-11 | Mitsubishi Metal Corp | Production of high-purity boron oxide powder |
| CN101003375A (en) * | 2007-01-19 | 2007-07-25 | 段贵华 | Preparing boric acid by complete cycled recrystal method |
| CN101412519A (en) * | 2008-10-29 | 2009-04-22 | 南京金美镓业有限公司 | Ion exchange and recrystallization combined preparation apparatus and method for high-purity boric acid |
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Denomination of invention: Preparation method of nuclear boric acid Effective date of registration: 20150215 Granted publication date: 20120201 Pledgee: Luo Baocheng Pledgor: Lu Xieying Registration number: 2015990000153 |