CN110846717A - Method for preparing sodium titanate whisker by using waste salt containing NaCl - Google Patents

Method for preparing sodium titanate whisker by using waste salt containing NaCl Download PDF

Info

Publication number
CN110846717A
CN110846717A CN201911197298.9A CN201911197298A CN110846717A CN 110846717 A CN110846717 A CN 110846717A CN 201911197298 A CN201911197298 A CN 201911197298A CN 110846717 A CN110846717 A CN 110846717A
Authority
CN
China
Prior art keywords
sodium titanate
preparing
precursor
nacl
waste
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.)
Pending
Application number
CN201911197298.9A
Other languages
Chinese (zh)
Inventor
于荟
赵利顺
于清跃
吴莉莉
唐棣
潘勇
张金龙
朱超凡
王森
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.)
Nanjing Polytechnic Institute
Original Assignee
Nanjing Polytechnic Institute
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 Nanjing Polytechnic Institute filed Critical Nanjing Polytechnic Institute
Priority to CN201911197298.9A priority Critical patent/CN110846717A/en
Publication of CN110846717A publication Critical patent/CN110846717A/en
Pending legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/16—Oxides
    • C30B29/22—Complex oxides
    • C30B29/32—Titanates; Germanates; Molybdates; Tungstates
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
    • C30B29/62—Whiskers or needles
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B9/00—Single-crystal growth from melt solutions using molten solvents
    • C30B9/04—Single-crystal growth from melt solutions using molten solvents by cooling of the solution
    • C30B9/08—Single-crystal growth from melt solutions using molten solvents by cooling of the solution using other solvents
    • C30B9/12—Salt solvents, e.g. flux growth

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention belongs to the field of treatment of industrial hazardous waste, and relates to a method for preparing sodium titanate whiskers by using waste salt containing NaCl to cooperatively treat the industrial hazardous waste. The invention provides a method for preparing sodium titanate whiskers by using waste salt containing NaCl, which comprises the following steps: the first step is as follows: preparing a precursor; the second step is that: and uniformly stirring the precursor, COD and mixed salt, adding a fluxing agent, roasting at high temperature, washing with deionized water, and drying to obtain the sodium titanate whisker. The invention adopts industrial hazardous waste containing NaCl as a reaction raw material, and prepares the sodium titanate whisker powder by a melting method, thereby preparing the sodium titanate whisker with low cost and excellent performance, realizing the resource and renewable utilization of the industrial hazardous waste, saving resources, reducing cost, simplifying process, reducing environmental pollution pressure, and the prepared whisker product has higher economic value and social value and is easy to realize industrialized production.

Description

Method for preparing sodium titanate whisker by using waste salt containing NaCl
Technical Field
The invention belongs to the field of treatment of industrial hazardous waste, and relates to a method for preparing sodium titanate whiskers by using waste salt containing NaCl.
Background
In the chemical production process, especially the pesticide production process, a large amount of high-salinity wastewater can be generated, the annual output of pesticides in China is large, and the wastewater is characterized in that: high organic matter concentration, complex components, high toxicity, difficult degradation, unstable water quality and the like. Such as the production of the herbicide glyphosate, produce high concentrations of phosphate and sodium chloride waste water. In addition, during the production process of preparing the soda ash by the ammonia-soda process, a large amount of high-salinity wastewater containing CaCl2 and NaCl soluble salts is generated, and the salt content in the wastewater still exceeds 2% after the wastewater is subjected to a relevant thermal concentration process. If the high-salinity wastewater is directly discharged, the high-salinity wastewater brings great harm to human health and environment, and the high-salinity wastewater is discharged after being treated, extra high cost is needed, and secondary pollution is also generated.
The whisker is a needle-shaped short fiber which is grown in a single crystal form under the condition of natural formation or artificial control, the diameter of the short fiber is submicron and nanometer size, the length-diameter ratio is generally more than 10, and the short fiber has excellent mechanical property, compatibility, smoothness, chemical stability and reusability and is widely applied due to the unique crystal structure. Among them, the sodium titanate whisker has low thermal conductivity and high infrared reflectivity, so that it can be used as excellent heat insulating material with low production cost. Industrial wastewater discharged by chemical plants in China every year contains a large amount of sodium chloride, and if the industrial wastewater is directly discharged, the industrial wastewater can permeate underground to increase the salt content of underground water, so that the water quality is influenced, the industrial wastewater cannot be drunk or irrigated in agriculture, and the environmental pollution to surrounding soil and water is serious.
At present, researchers adopt industrial pure sodium compounds and titanium compound solid powder as raw materials for preparing sodium titanate whiskers, so that the cost is high; in industry, inorganic solid waste generated in the production process of a plurality of coal chemical industry and pharmaceutical industry generally contains mixed salts of NaCl, Na2SO4 and KCl, belongs to the category of industrial hazardous waste, and brings great harm to human health and environment if directly discharged into the environment; if the dangerous waste treatment is carried out, extra economic burden is increased.
Therefore, the invention aims to synthesize the sodium titanate whisker by using industrial waste salt (containing NaCl) as a molten salt type raw material so as to prepare low-cost industrial powder and a method for cooperatively treating industrial hazardous waste. The invention can not only obtain the material with high added value, but also remove the organic matters in the waste salt through high temperature, and can also prepare industrial salt through further separation.
Disclosure of Invention
1. The technical problem to be solved is as follows:
inorganic solid waste generated in the production process of coal chemical industry and pharmaceutical industry generally contains mixed salts NaCl, Na2SO4 and KCl, belongs to the category of industrial hazardous waste, and brings great harm to human health and environment if directly discharged into the environment; if the dangerous waste treatment is carried out, extra economic burden is increased.
2. The technical scheme is as follows:
in order to solve the problems, the invention provides a method for preparing sodium titanate whiskers by using NaCl-containing waste salt, which comprises the following steps: the first step is as follows: preparing a precursor; the second step is that: and uniformly stirring the precursor, COD and mixed salt, adding a fluxing agent, roasting at high temperature, washing with deionized water, and drying to obtain the sodium titanate whisker.
The precursor is a titanium dioxide precursor.
The preparation method of the titanium dioxide precursor comprises the following steps: tetrabutyl titanate is used as a raw material, hydrothermal temperature is 80-220 ℃ for 2-6h, heat preservation is carried out for 10-40h in hydrothermal reaction, then centrifugation is carried out at a centrifugation speed of 6000-.
The mixed salt is NaCl and Na2SO4Mixing the salts.
In the second step, the NaCl and Na2SO4Mass ratio: 0.5-5, mass ratio of COD to mixed salt: 0.5-5.
In the second step, the roasting temperature is as follows: 600 ℃ and 1200 ℃, the roasting time is 2-12h,
in the second step, the drying temperature is 80-100 ℃.
In the second step, deionized water is used for washing for 1-2 h.
The cosolvent is one or a mixture of sodium carbonate, sodium sulfate, sodium chloride and boric acid.
The mass of the cosolvent is 1-3% of the total mass.
3. Has the advantages that:
the invention adopts industrial hazardous waste containing NaCl as a reaction raw material, and prepares the sodium titanate whisker powder by a melting method, thereby preparing the sodium titanate whisker with low cost and excellent performance, realizing the resource and renewable utilization of the industrial hazardous waste, saving resources, reducing cost, simplifying process, reducing environmental pollution pressure, and the prepared whisker product has higher economic value and social value and is easy to realize industrialized production.
Detailed Description
The present invention will be described in detail below with reference to examples.
Example 1
The preparation method of the titanium dioxide precursor comprises the steps of taking tetrabutyl titanate as a raw material, conducting hydrothermal reaction at 80 ℃ for 6 hours, conducting heat preservation for 40 hours in the hydrothermal reaction, then conducting centrifugation at 8000r/min for 2 hours, washing with deionized water for 2 hours, and then conducting drying at 100 ℃ to obtain the titanium dioxide precursor.
Example 2
The preparation method of the titanium dioxide precursor comprises the following steps: tetrabutyl titanate is used as a raw material, hydrothermal temperature is 150 ℃ for 4h, heat preservation is carried out for 20h in hydrothermal reaction, then centrifugation is carried out at 6000r/min for 1.5h, deionized water is used for washing for 1.5h, and drying is carried out at 90 ℃ to obtain the titanium dioxide precursor.
Example 3
The preparation method of the titanium dioxide precursor comprises the following steps: tetrabutyl titanate is used as a raw material, the hydrothermal temperature is 220 ℃ for 2 hours, the hydrothermal reaction is carried out for 10 hours, then the titanium dioxide precursor is obtained by centrifuging at a centrifugal speed of 9000r/min for 1 hour, washing with deionized water for 1 hour and drying at a temperature of 80 ℃.
Example 4
A titanium dioxide precursor was produced according to any one of the methods in examples 1 to 3, and NaCl and Na were prepared in a mass ratio of 0.32SO4COD and mixed salt in a mass ratio of 0.3.
Uniformly stirring the titanium dioxide precursor, COD and mixed salt, wherein the mixed salt is NaCl and Na2SO4And (4) mixing. Adding any one of sodium carbonate, sodium sulfate, sodium chloride and boric acid, roasting at 900 ℃ for 8h, washing with deionized water for 1.5h, and drying at 90 ℃ to obtain the sodium titanate whisker.
Example 5
A titanium dioxide precursor was obtained according to any one of the methods in examples 1 to 3, and NaCl and Na were prepared in a mass ratio of 0.52SO4COD and mixed salt in a mass ratio of 5.
Uniformly stirring a titanium dioxide precursor, COD (chemical oxygen demand) and mixed salt, wherein the mixed salt is NaCl and Na2SO4And (4) mixing. Adding any two of sodium carbonate, sodium sulfate, sodium chloride and boric acid, mixing, roasting at 800 deg.C for 12 hr, washing with deionized water for 2 hr, and drying at 100 deg.C to obtain sodium titanate whisker.
Example 6
A titanium dioxide precursor was produced according to any one of the methods in examples 1 to 3, and NaCl and Na were prepared in a mass ratio of 52SO4The mass ratio of the COD to the mixed salt is 0.5.
Uniformly stirring a titanium dioxide precursor, COD (chemical oxygen demand) and mixed salt, wherein the mixed salt is NaCl and Na2SO4And (4) mixing. Adding any three to four of sodium carbonate, sodium sulfate, sodium chloride and boric acid, mixing, roasting at 1200 deg.C for 2 hr, washing with deionized water for 1 hr, and drying at 80 deg.C to obtain sodium titanate crystalAnd (5) whiskers are needed.
The embodiment shows that the method provided by the invention utilizes the relevant components in the industrial hazardous waste, realizes the resource recycling of the industrial hazardous waste, saves resources, reduces the cost, simplifies the process, relieves the environmental pollution pressure, effectively removes COD in the process of preparing the crystal whisker, and the prepared crystal whisker product has higher economic value and social value and is easy to realize industrial production.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (10)

1. A method for preparing sodium titanate whiskers by using NaCl-containing waste salt comprises the following steps: the first step is as follows: preparing a precursor; the second step is that: and uniformly stirring the precursor, COD and mixed salt, adding a fluxing agent, roasting at high temperature, washing with deionized water, and drying to obtain the sodium titanate whisker.
2. The method of claim 1, wherein: the precursor is a titanium dioxide precursor.
3. The method of claim 2, wherein: the preparation method of the titanium dioxide precursor comprises the following steps: tetrabutyl titanate is used as a raw material, hydrothermal temperature is 80-220 ℃ for 2-6h, heat preservation is carried out for 10-40h in hydrothermal reaction, then centrifugation is carried out at a centrifugation speed of 6000-.
4. The method of claim 1, wherein: the mixed salt is NaCl and Na2SO4And (4) mixing.
5. The method as claimed in any one of claims 1 to 4The method is characterized in that: in the second step, the NaCl and Na2SO4Mass ratio: 0.5-5, mass ratio of COD to mixed salt: 0.5-5.
6. The method of any one of claims 1-4, wherein: in the second step, the roasting temperature is as follows: 600 ℃ and 1200 ℃, and the roasting time is 2-12 h.
7. The method of any one of claims 1-4, wherein: in the second step, the drying temperature is 80-100 ℃.
8. The method of any one of claims 1-4, wherein: in the second step, deionized water is used for washing for 1-2 h.
9. The method of any one of claims 1-4, wherein: the cosolvent is one or a mixture of sodium carbonate, sodium sulfate, sodium chloride and boric acid.
10. The method of claim 9, wherein: the mass of the cosolvent is 1-3% of the total mass.
CN201911197298.9A 2019-11-29 2019-11-29 Method for preparing sodium titanate whisker by using waste salt containing NaCl Pending CN110846717A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201911197298.9A CN110846717A (en) 2019-11-29 2019-11-29 Method for preparing sodium titanate whisker by using waste salt containing NaCl

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201911197298.9A CN110846717A (en) 2019-11-29 2019-11-29 Method for preparing sodium titanate whisker by using waste salt containing NaCl

Publications (1)

Publication Number Publication Date
CN110846717A true CN110846717A (en) 2020-02-28

Family

ID=69606119

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201911197298.9A Pending CN110846717A (en) 2019-11-29 2019-11-29 Method for preparing sodium titanate whisker by using waste salt containing NaCl

Country Status (1)

Country Link
CN (1) CN110846717A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114774701A (en) * 2022-06-20 2022-07-22 国能龙源环保有限公司 Resource utilization method of industrial waste salt and waste denitration catalyst

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101117728A (en) * 2006-08-04 2008-02-06 上海秀普复合材料有限公司 Method for synthesizing sodium titanate whisker
CN101275276A (en) * 2007-12-25 2008-10-01 山东大学 Preparation for sodium titanate crystal whisker
CN101363136A (en) * 2007-08-10 2009-02-11 上海晶须复合材料制造有限公司 Synthesis method of sodium hexatitanate whisker
CN108620053A (en) * 2017-07-17 2018-10-09 中国地质大学（北京） A kind of method that molten-salt growth method prepares meta-titanium perborate-potassium tetratitanate composite catalyzing material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101117728A (en) * 2006-08-04 2008-02-06 上海秀普复合材料有限公司 Method for synthesizing sodium titanate whisker
CN101363136A (en) * 2007-08-10 2009-02-11 上海晶须复合材料制造有限公司 Synthesis method of sodium hexatitanate whisker
CN101275276A (en) * 2007-12-25 2008-10-01 山东大学 Preparation for sodium titanate crystal whisker
CN108620053A (en) * 2017-07-17 2018-10-09 中国地质大学（北京） A kind of method that molten-salt growth method prepares meta-titanium perborate-potassium tetratitanate composite catalyzing material

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
汪多仁等: "《绿色化工助剂》", 1 January 2006, 科学技术文献出版社 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114774701A (en) * 2022-06-20 2022-07-22 国能龙源环保有限公司 Resource utilization method of industrial waste salt and waste denitration catalyst
CN114774701B (en) * 2022-06-20 2022-09-06 国能龙源环保有限公司 Resource utilization method of industrial waste salt and waste denitration catalyst
WO2023246080A1 (en) * 2022-06-20 2023-12-28 国能龙源环保有限公司 Method for recycling industrial waste salt and waste denitration catalyst

Similar Documents

Publication Publication Date Title
Gao et al. Utilization of distiller waste and residual mother liquor to prepare precipitated calcium carbonate
CN103922378B (en) Method for preparing high-purity metastable vaterite calcium carbonate from gypsum
CN107460759B (en) Rapid purification method of nano-cellulose suspension
CN101066771A (en) Microwave radiation process for producing potassium sulfate
CN110846717A (en) Method for preparing sodium titanate whisker by using waste salt containing NaCl
CN1124784C (en) Biological Pesticide prepared with the extraction from xianggu mushroom leftover and the preparation process
CN110128213A (en) A method of liquid fertilizer is produced using beer waste yeast
CN103626210A (en) Method for preparing magnesium hydroxide and chlorine by coupling magnesium chloride reactive crystallization and electrolysis
CN1369445A (en) Process for treating sewage to generate active mud and extract protein
CN107473244B (en) A kind of method that spodumene prepares lithium carbonate by-product potassium type zeolite
CN105858676A (en) Production method for coproducing sodium silicate and sodium fluoride
CN103121697B (en) Pure silicon ANA-type zeolite molecular sieve and preparation method thereof
CN112047401B (en) Method for thickening and refining seawater by using sodium sulfate
CN101648708B (en) Preparing method of high-purity carbon dioxide
CN106638087A (en) Natural high-crystallinity-degree plant cellulose and preparation method thereof
CN111547747A (en) Process for producing potassium nitrate by using brine as raw material
CN103834997B (en) Method for preparing calcium carbonate whisker from saccharose by assisting hydrothermal process
CN111215430A (en) Alkaline residue utilization method for separating calcium and magnesium by phase transfer method
CN106430233B (en) A kind of Na2CO3The method that-NaOH mixing alkali fusion activation potassium bearing rock produces low-silicon X-shaped molecular screen
CN100595254C (en) Method for preparing amphoteric ion polymer fluid loss additive
CN1032150A (en) Process for producing flocculant of polymeric aluminium chloride
CN1246259C (en) Magnesium-ammonium mixed salt steaming-boiling agent for producing culture paper in which the black liquid is directly used as organic fertilizer
CN114749156B (en) Method for preparing demethylated lignin adsorption material by ball milling
CN103626596B (en) Method for preparing fertilizer from activated sludge
CN116020400A (en) Preparation method of modified fly ash for treating ammonia nitrogen wastewater

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
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20200228