CN110803709B - Centrifugal spray drying preparation method of anhydrous lithium hydroxide - Google Patents

Centrifugal spray drying preparation method of anhydrous lithium hydroxide Download PDF

Info

Publication number
CN110803709B
CN110803709B CN201911125117.1A CN201911125117A CN110803709B CN 110803709 B CN110803709 B CN 110803709B CN 201911125117 A CN201911125117 A CN 201911125117A CN 110803709 B CN110803709 B CN 110803709B
Authority
CN
China
Prior art keywords
lithium hydroxide
nitrogen
impurities
drying tower
atomizer
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201911125117.1A
Other languages
Chinese (zh)
Other versions
CN110803709A (en
Inventor
吴文斌
丁海云
孙雪云
龚明明
郭国龙
苗强
王春叶
杜桂荣
周京霞
陈琳
熊国鸿
曹淑琴
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Beijing Research Institute of Chemical Engineering and Metallurgy of CNNC
Original Assignee
Beijing Research Institute of Chemical Engineering and Metallurgy of CNNC
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Beijing Research Institute of Chemical Engineering and Metallurgy of CNNC filed Critical Beijing Research Institute of Chemical Engineering and Metallurgy of CNNC
Priority to CN201911125117.1A priority Critical patent/CN110803709B/en
Publication of CN110803709A publication Critical patent/CN110803709A/en
Application granted granted Critical
Publication of CN110803709B publication Critical patent/CN110803709B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D15/00—Lithium compounds
    • C01D15/02—Oxides; Hydroxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D1/00—Evaporating
    • B01D1/16—Evaporating by spraying
    • B01D1/18—Evaporating by spraying to obtain dry solids
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

The invention belongs to the technical field of chemical substance preparationIn particular to a centrifugal spray drying preparation method of anhydrous lithium hydroxide. In the technical scheme of the invention, under the protection of nitrogen, lithium hydroxide monohydrate (lithium hydroxide) added with impurities7LiOH is subjected to spray centrifugal drying and condensation separation to remove water, and the nano anhydrous lithium hydroxide (A), (B) is prepared7LiOH) powder in which the added impurities are distributed homogeneously, the lithium hydroxide7LiOH) powder has uniform impurity distribution, and can be used as lithium hydroxide (lithium hydroxide) after system detection and verification7LiOH) standard substance.

Description

Centrifugal spray drying preparation method of anhydrous lithium hydroxide
Technical Field
The invention belongs to the technical field of chemical substance preparation, and particularly relates to a centrifugal spray drying preparation method of anhydrous lithium hydroxide.
Background
Lithium hydroxide for nuclear power7LiOH) is enriched in lithium7Li(7Li/Total Li>99.9%) due to7Li has the smallest neutron cross-section, so lithium hydroxide (7LiOH) is used to adjust the pH of the primary water of the pressurized water reactor. The pressurized water reactor uses water as a primary coolant, circulates in a high-temperature high-pressure and strong radiation field, and carries out a series of reactions besides heat carrying and moderating neutrons: water and therein Neutron activation reactions of impurities, radiolysis of water, corrosion of materials by water and activation, migration and deposition of corrosion products, escape of fission products from damaged fuel elements and their transfer with coolant, etc. Although the surfaces of the equipment and the pipeline of the primary loop coolant system are made of stainless steel materials, oxygen or other harmful substances contained in water can corrode the materials, the service life of the equipment is shortened, and solid corrosion products become new radiation sources after being irradiated by neutrons. The pH value in the coolant has great influence on the corrosion rate of the material, and the corrosion rate of the stainless steel material is the lowest when water is in weak alkalinity. By controlling lithium hydroxide7The content of LiOH is used for adjusting the alkalescence of water so as to avoid or reduce the corrosion of materials, and lithium hydroxide7LiOH) has strict index requirements on impurities in the product. To ensure nuclear pure lithium hydroxide (7The accuracy of analysis and test results of various impurity elements in the LiOH) application process needs to develop lithium hydroxide (LiOH)7LiOH) (abundant Li-7) standard substance, nuclear pure lithium hydroxide (II)7LiOH) production application process and analytical process.
And currently there is no anhydrous lithium hydroxide ( 7LiOH), there is a need to develop a centrifugal spray-drying preparation method of anhydrous lithium hydroxide, thereby solving the above problems.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a centrifugal spray drying preparation method of anhydrous lithium hydroxide so as to meet the requirement of lithium hydroxide7The requirements of quantity transmission, evaluation analysis method, personnel assessment and the like for detecting impurity elements in LiOH) ensure that lithium hydroxide (lithium hydroxide)7LiOH) quality of the product.
In order to realize the purpose, the invention adopts the technical scheme that:
a centrifugal spray drying preparation method of anhydrous lithium hydroxide comprises the following steps:
(1) determining a preparation system
(2) Determination of specific Process steps
Dissolving high-purity lithium hydroxide monohydrate and impurities in a plastic barrel by using deionized water at room temperature to form mixed solution containing lithium hydroxide and impurities;
secondly, the mixed liquid is sucked by a peristaltic pump and is sent to a high-speed centrifugal atomizer at the top of the drying tower, and meanwhile, nitrogen heated by an electric heater is blown into the high-speed centrifugal atomizer;
thirdly, under the action of centrifugal force, the mixed liquid in the atomizer forms a fog group and is sprayed out from the spray holes of the atomizing disk;
driven by nitrogen in the step (2), quickly evaporating water in the fog group in the step (2) to dryness to form dry powder;
Fifthly, the dry powder formed in the step (2) is sucked into a cloth bag collector through a discharge pipe for collection;
sixthly, the nitrogen containing the water vapor enters a condenser, wherein the water vapor is condensed into water to be discharged, and the nitrogen enters the heating device again through a pipeline by the exhaust fan to realize circulation.
Further, in the above-mentioned centrifugal spray-drying preparation method of anhydrous lithium hydroxide, in the step (1), the components of the preparation system are specifically as follows:
the peristaltic pump is connected with the atomizer through a silicone tube;
the atomizer is arranged at the upper part of the drying tower and is connected with the drying tower;
the electric heater is arranged on the side of the drying tower;
conveying the nitrogen heated by the electric heater into a drying tower through a hot air distributor;
the lower outlet of the drying tower is connected with the filter bag separator through a pipeline;
gas-solid separation is realized in the filter bag separator;
the lower part of the filter bag separator is provided with a product collecting tank;
the upper part of the filter bag separator is connected with the top of the condenser through a pipeline, and nitrogen and water vapor enter the condenser through the pipeline;
the condensed water enters a solvent collector at the lower end of the condenser and is discharged through a discharge port, and the condensed nitrogen is recycled by an exhaust fan.
Further, a centrifugal spray of anhydrous lithium hydroxide as described above The preparation method comprises the step (2), wherein in the step (2), the impurities comprise Ca, Pb, Zn, Cl and F-、SO4 2-。
Further, in the above-mentioned centrifugal spray-drying preparation method of anhydrous lithium hydroxide, in the (2) part (r), impurities are added to the highly pure lithium hydroxide monohydrate by the following form: ca (NO)3)2、Pb(NO3)2、Zn(NO3)2、HCl、HF、H2SO4。
Further, the centrifugal spray drying preparation method of anhydrous lithium hydroxide comprises the following steps of (2), in the step (2), adding 10-500 mg of impurities of Ca, Pb and Zn into each kilogram of lithium hydroxide; adding Cl and F to each kilogram of lithium hydroxide-、SO4 2-All 50-1000 mg.
Further, according to the centrifugal spray drying preparation method of anhydrous lithium hydroxide, in the step (2), the mixed solution is sucked into a high-speed centrifugal atomizer at the top of the drying tower through a peristaltic pump, and nitrogen heated to 180-300 ℃ by an electric heater is blown into the high-speed centrifugal atomizer.
Further, the centrifugal spray drying preparation method of anhydrous lithium hydroxide comprises the step (2) and the flow rate of nitrogen is 1-3 Nm3The pressure of nitrogen is 1-3 kPa.
Further, in the centrifugal spray drying preparation method of anhydrous lithium hydroxide, in the third step (2), the centrifugal force is provided by a centrifugal disc with the rotation speed of 10000-20000 revolutions per minute.
The technical scheme of the invention has the beneficial effects that:
1) spray drying technique using nitrogen gas circulation protection from lithium hydroxide7The LiOH solution is directly prepared into anhydrous lithium hydroxide (lithium hydroxide) with similar chemical components in one step7LiOH) powder, to achieve different contents of impurity elements in anhydrous lithium hydroxide7LiOH) are uniformly distributed in the preparation process.
2) Can continuously complete anhydrous lithium hydroxide7LiOH) standard substance candidates, improving the working environment.
3) Breaks through the conventional method of preparing standard substances by physical pulverization.
Detailed Description
The technical solution of the present invention will be described in detail with reference to the following specific examples.
The invention relates to a centrifugal spray drying preparation method of anhydrous lithium hydroxide, which comprises the following steps:
(1) determining a preparation system
The components of the preparation system are as follows:
the peristaltic pump is connected with the atomizer through a silicone tube;
the atomizer is arranged at the upper part of the drying tower and is connected with the drying tower;
the electric heater is arranged on the side of the drying tower;
conveying the nitrogen heated by the electric heater into a drying tower through a hot air distributor;
the lower outlet of the drying tower is connected with the filter bag separator through a pipeline;
gas-solid separation is realized in the filter bag separator;
the lower part of the filter bag separator is provided with a product collecting tank;
The upper part of the filter bag separator is connected with the top of the condenser through a pipeline, and nitrogen and water vapor enter the condenser through the pipeline;
the condensed water enters a solvent collector at the lower end of the condenser and is discharged through a discharge port, and the condensed nitrogen is recycled by an exhaust fan;
(2) determination of specific Process steps
Dissolving high-purity lithium hydroxide monohydrate and impurities in a plastic barrel by using deionized water at room temperature to form mixed solution containing lithium hydroxide and impurities;
the impurities include Ca, Pb, Zn, Cl, F-、SO4 2-；
The impurities are added to the high purity lithium hydroxide monohydrate by the following form: ca (NO)3)2、Pb(NO3)2、Zn(NO3)2、HCl、HF、H2SO4；
Each kilogram of lithium hydroxide is added with 10-500 mg of impurities of Ca, Pb and Zn; adding Cl and F to each kilogram of lithium hydroxide-、SO4 2-50-1000 mg;
secondly, sucking the mixed liquid into a high-speed centrifugal atomizer at the top of the drying tower by a peristaltic pump, and blowing nitrogen heated to 180-300 ℃ by an electric heater into the high-speed centrifugal atomizer;
the flow rate of nitrogen is 1-3 Nm3The pressure of nitrogen is 1-3 kPa;
thirdly, under the action of centrifugal force provided by a centrifugal disc with the rotating speed of 10000-20000 revolutions per minute, mixed liquid in the atomizer forms a fog group and is sprayed out from spray holes of the atomizing disc;
driven by nitrogen in the step (2), quickly evaporating water in the fog group in the step (2) to dryness to form dry powder;
Fifthly, the dry powder formed in the step (2) is sucked into a cloth bag collector through a discharge pipe for collection;
sixthly, the nitrogen containing the water vapor enters a condenser, wherein the water vapor is condensed into water to be discharged, and the nitrogen enters the heating device again through a pipeline by the exhaust fan to realize circulation.
In the technical scheme of the invention, under the protection of nitrogen, lithium hydroxide monohydrate (lithium hydroxide) added with impurities7LiOH is subjected to spray centrifugal drying and condensation separation to remove water, and the nano anhydrous lithium hydroxide (A), (B) is prepared7LiOH) powder in which the added impurities are distributed homogeneously, the lithium hydroxide7LiOH) powder has uniform impurity distribution, and can be used as lithium hydroxide (lithium hydroxide) after system detection and verification7LiOH) standard substance.

Claims (1)

1. A centrifugal spray drying preparation method of anhydrous lithium hydroxide is characterized by comprising the following steps:
(1) determining a preparation system
(2) Determination of specific Process steps
Dissolving high-purity lithium hydroxide monohydrate and impurities in a plastic barrel by using deionized water at room temperature to form mixed solution containing lithium hydroxide and impurities;
secondly, the mixed liquid is sucked by a peristaltic pump and is sent to a high-speed centrifugal atomizer at the top of the drying tower, and meanwhile, nitrogen heated by an electric heater is blown into the high-speed centrifugal atomizer;
Thirdly, under the action of centrifugal force, the mixed liquid in the atomizer forms a fog group and is sprayed out from the spray holes of the atomizing disk;
driven by nitrogen in the step (2), quickly evaporating water in the fog group in the step (2) to dryness to form dry powder;
fifthly, the dry powder formed in the step (2) is sucked into a cloth bag collector through a discharge pipe for collection;
sixthly, nitrogen containing water vapor enters a condenser, wherein the water vapor is condensed into water to be discharged, and the nitrogen enters the heating device again through a pipeline by the exhaust fan to realize circulation;
in the step (1), each part of the preparation system is as follows:
the peristaltic pump is connected with the atomizer through a silicone tube;
the atomizer is arranged at the upper part of the drying tower and is connected with the drying tower;
the electric heater is arranged on the side of the drying tower;
conveying the nitrogen heated by the electric heater into a drying tower through a hot air distributor;
the lower outlet of the drying tower is connected with the filter bag separator through a pipeline;
gas-solid separation is realized in the filter bag separator;
the lower part of the filter bag separator is provided with a product collecting tank;
the upper part of the filter bag separator is connected with the top of the condenser through a pipeline, and nitrogen and water vapor enter the condenser through the pipeline;
the condensed water enters a solvent collector at the lower end of the condenser and is discharged through a discharge port, and the condensed nitrogen is recycled by an exhaust fan;
In the step (2), the impurities include Ca, Pb, Zn, Cl and F-、SO4 2-(ii) a The impurities are added to the high purity lithium hydroxide monohydrate by the following form: ca (NO)3)2、Pb(NO3)2、Zn(NO3)2、HCl、HF、H2SO4(ii) a Each kilogram of lithium hydroxide is added with 10-500 mg of impurities of Ca, Pb and Zn; adding Cl and F to each kilogram of lithium hydroxide-、SO4 2-50-1000 mg;
in the step (2), the mixed liquid is sucked into a high-speed centrifugal atomizer at the top of the drying tower by a peristaltic pump, and nitrogen heated to 180-300 ℃ by an electric heater is blown into the high-speed centrifugal atomizer;
in the step (2), the flow rate of nitrogen is 1-3 Nm3The pressure of nitrogen is 1-3 kPa;
in the third step (2), centrifugal force is provided by a centrifugal disc with the rotating speed of 10000-20000 revolutions per minute.
CN201911125117.1A 2019-11-18 2019-11-18 Centrifugal spray drying preparation method of anhydrous lithium hydroxide Active CN110803709B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201911125117.1A CN110803709B (en) 2019-11-18 2019-11-18 Centrifugal spray drying preparation method of anhydrous lithium hydroxide

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201911125117.1A CN110803709B (en) 2019-11-18 2019-11-18 Centrifugal spray drying preparation method of anhydrous lithium hydroxide

Publications (2)

Publication Number Publication Date
CN110803709A CN110803709A (en) 2020-02-18
CN110803709B true CN110803709B (en) 2022-03-22

Family

ID=69490250

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201911125117.1A Active CN110803709B (en) 2019-11-18 2019-11-18 Centrifugal spray drying preparation method of anhydrous lithium hydroxide

Country Status (1)

Country Link
CN (1) CN110803709B (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111943235A (en) * 2020-06-29 2020-11-17 深圳石墨烯创新中心有限公司 Preparation process of battery-grade anhydrous lithium hydroxide
CN112216834B (en) * 2020-10-29 2021-08-03 湖南永杉锂业有限公司 Method for preparing modified anhydrous lithium hydroxide by spray coating

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109502611A (en) * 2018-11-16 2019-03-22 湖南众德新材料科技有限公司 A kind of device preparing lithium hydroxide micro nano powder
CN109553118A (en) * 2018-12-19 2019-04-02 江西赣锋锂业股份有限公司 A kind of method of industrial production anhydrous lithium hydroxide ball
CN110255577A (en) * 2019-06-05 2019-09-20 核工业北京化工冶金研究院 The pure grade boric acid standard substance preparation process of one seed nucleus

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8895468B2 (en) * 2011-09-20 2014-11-25 Basf Corporation Chromia alumina catalysts for alkane dehydrogenation

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109502611A (en) * 2018-11-16 2019-03-22 湖南众德新材料科技有限公司 A kind of device preparing lithium hydroxide micro nano powder
CN109553118A (en) * 2018-12-19 2019-04-02 江西赣锋锂业股份有限公司 A kind of method of industrial production anhydrous lithium hydroxide ball
CN110255577A (en) * 2019-06-05 2019-09-20 核工业北京化工冶金研究院 The pure grade boric acid standard substance preparation process of one seed nucleus

Also Published As

Publication number Publication date
CN110803709A (en) 2020-02-18

Similar Documents

Publication Publication Date Title
CN110803709B (en) Centrifugal spray drying preparation method of anhydrous lithium hydroxide
CN102583459B (en) Process for preparing magnesium sulfate monohydrate by using water-containing magnesium sulfate heptahydrate
CN106166396A (en) A kind of energy-saving closed cycle spray drying system
CN102607247B (en) Spray dryer
CN108686608A (en) Bushing type I-131 destructive distillation absorbers
CN108619908A (en) A kind of horizontal dual temperature area I-131 destructive distillation devices
CN209685657U (en) A kind of polymer purification separation integrated device
CN108686606A (en) A kind of heap shines TeO2Produce the destructive distillation device of iodine -131
CN109626468A (en) The processing system of desulfurization wastewater
JP2012161770A (en) Means for disposing waste liquid and method for disposing and recovering waste liquid
CN206837530U (en) A kind of vacuum evaporation device for being used to reclaim full heat and latent heat
CN108654377A (en) A kind of ventilation type Na131I preparation destructive distillation devices
CN211963099U (en) Closed-cycle centrifugal spray drying equipment
CN104326519B (en) Evaporating condensation type sea water desalinating unit
CN114642938A (en) UO prepared by uranyl nitrate atomization drying pyrolysis denitration3Method for treating tail gas
CN107584695A (en) A kind of damaged tire low-temperature atmosphere-pressure thermal cracking production technology
CN106906016A (en) A kind of energy-efficient pretreatment process method for the gas that generates electricity
CN217745738U (en) Manufacturing equipment of industrial pharmaceutical sodium dodecyl sulfate
CN217211724U (en) But gas-solid separation's atmosphere pollutant collection system
CN217211723U (en) Continuous collection system of atmospheric aerosol liquid phase
CN211435119U (en) Micromolecule atomization drying crystallization equipment
CN209271106U (en) A kind of heating conduit anti-flammability gas circulation desorption organic waste gas recycling system
CN103011244B (en) Method for preparing high soda ash type copper carbonate by adopting duplex centrifugal film evaporator
CN208482463U (en) A kind of I-131 production destructive distillation absorber
CN205856359U (en) A kind of NMP in working procedure of coating lithium ion cell recycle device

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant