CN115896484A - Molybdenum removal detection method for high-molybdenum tungsten concentrate - Google Patents
Molybdenum removal detection method for high-molybdenum tungsten concentrate Download PDFInfo
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- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 38
- 239000011733 molybdenum Substances 0.000 title claims abstract description 38
- 239000012141 concentrate Substances 0.000 title claims abstract description 33
- 238000001514 detection method Methods 0.000 title claims abstract description 26
- 239000000440 bentonite Substances 0.000 claims abstract description 47
- 229910000278 bentonite Inorganic materials 0.000 claims abstract description 47
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims abstract description 47
- 229920001661 Chitosan Polymers 0.000 claims abstract description 42
- 239000000706 filtrate Substances 0.000 claims abstract description 38
- 239000003607 modifier Substances 0.000 claims abstract description 38
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 29
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000001556 precipitation Methods 0.000 claims abstract description 22
- 230000004048 modification Effects 0.000 claims abstract description 21
- 238000012986 modification Methods 0.000 claims abstract description 21
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 16
- 239000010937 tungsten Substances 0.000 claims abstract description 16
- 238000004073 vulcanization Methods 0.000 claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 82
- 238000003756 stirring Methods 0.000 claims description 56
- 239000005543 nano-size silicon particle Substances 0.000 claims description 36
- 235000012239 silicon dioxide Nutrition 0.000 claims description 36
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 28
- 238000000227 grinding Methods 0.000 claims description 21
- VQEHIYWBGOJJDM-UHFFFAOYSA-H lanthanum(3+);trisulfate Chemical compound [La+3].[La+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O VQEHIYWBGOJJDM-UHFFFAOYSA-H 0.000 claims description 21
- 239000000654 additive Substances 0.000 claims description 18
- 230000000996 additive effect Effects 0.000 claims description 18
- 238000002360 preparation method Methods 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 14
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 14
- 235000010413 sodium alginate Nutrition 0.000 claims description 14
- 239000000661 sodium alginate Substances 0.000 claims description 14
- 229940005550 sodium alginate Drugs 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- 239000000047 product Substances 0.000 claims description 13
- 239000000377 silicon dioxide Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 7
- 239000002841 Lewis acid Substances 0.000 claims description 7
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 7
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 7
- 239000002041 carbon nanotube Substances 0.000 claims description 7
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 7
- OKTJSMMVPCPJKN-YPZZEJLDSA-N carbon-10 atom Chemical compound [10C] OKTJSMMVPCPJKN-YPZZEJLDSA-N 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 239000007822 coupling agent Substances 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 150000007517 lewis acids Chemical class 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 238000002715 modification method Methods 0.000 claims description 7
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 7
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 4
- 238000005486 sulfidation Methods 0.000 claims 1
- 239000002244 precipitate Substances 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 13
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 6
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 229910001145 Ferrotungsten Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to the technical field of molybdenum removal detection, and particularly discloses a molybdenum removal detection method for high-molybdenum tungsten concentrate, which comprises the following steps of: preparing tungsten concentrate into tungstate solution, and then carrying out vulcanization precipitation modification treatment; preparing an auxiliary modifier for bentonite; and adding the bentonite auxiliary modifier into 3-5 times of the chitosan modifying solution to obtain a filtrate treating agent. According to the molybdenum removal detection method, the tungstate solution is precipitated and vulcanized, the precipitate is firstly carried out, then the bentonite auxiliary modifier is matched with the chitosan modified solution, and the filtrate is further filtered, so that the molybdenum adsorption treatment efficiency is improved.
Description
Technical Field
The invention relates to the technical field of molybdenum removal detection, in particular to a molybdenum removal detection method for high-molybdenum tungsten concentrate.
Background
Tungsten belongs to rare elements and comprises ferrotungsten concentrate and calcium tungstate concentrate, the content of tungsten in the crust is only 0.8%, the tungsten reserves in China account for about 55% of the total reserves in the world, and the tungsten reserves are the top. Tungsten concentrate is produced in northwest, northwest and southwest, and particularly tungsten ore is produced in the south mountain range from southwest to southwest in the west, hunan, guangdong, jiangxi and east to Fujian. The south of the West river is the most concentrated, and the large and small mines reach hundreds of places, and the Daji mountain, the Xihua mountain, the Meishan mountain, the Pangushan and the like are famous tungsten mines in the world.
In the existing molybdenum removal detection method, tungsten concentrate with high molybdenum content is difficult to settle and treat cleanly, so that the detection efficiency is influenced.
Disclosure of Invention
In view of the defects of the prior art, the present invention aims to provide a method for detecting molybdenum removal of high-molybdenum tungsten concentrate, so as to solve the problems in the background art.
The technical scheme adopted by the invention for solving the technical problem is as follows:
the invention provides a molybdenum removal detection method for high-molybdenum tungsten concentrate, which comprises the following steps of:
the method comprises the following steps: preparing tungsten concentrate into tungstate solution, and then carrying out vulcanization precipitation modification treatment;
step two: preparing an auxiliary modifier for bentonite;
step three: adding bentonite auxiliary modifier into 3-5 times of chitosan modified solution to obtain filtrate treating agent;
step four: stirring the filtrate modified by the precipitation in the step one by using a filtrate treating agent for reaction treatment, and ending the stirring;
step five: and finally, filtering, washing and drying the filtrate, and finally detecting the content of molybdenum in the residual filtrate.
Preferably, the tungstate solution is 10-20% by mass of sodium tungstate solution.
Preferably, the method for the modification treatment of the sulfide precipitation comprises the following steps: adding hexadecyl trimethyl ammonium bromide 10-15% of tungstate solution, stirring at 450-550r/min for 20-30min, and stirring.
Preferably, the preparation method of the bentonite auxiliary modifier comprises the following steps:
s1: adding bentonite into a hydrochloric acid solution according to the weight ratio of 1;
s2: adding lanthanum sulfate into a sodium alginate solution with the mass fraction of 10-20% which is 3-5 times that of the lanthanum sulfate, and adding modified nano silicon dioxide with the mass fraction of 2-5% of the lanthanum sulfate to obtain a nano silicon dioxide additive;
s3: adding the nano silicon dioxide additive into S1 according to the weight ratio of 1;
s4: and (4) carrying out thermal improvement treatment on the product of the S3, and finishing the treatment to obtain the bentonite auxiliary modifier.
Preferably, the mass fraction of the hydrochloric acid solution is 5-10%; the mass fraction of the sodium alginate solution is 10-20%.
Preferably, the silane coupling agent is a coupling agent KH560.
Preferably, the modification method of the modified nano-silica comprises the following steps:
adding 15-20 parts of nano silicon dioxide into 2-5 parts of grinding agent, grinding at the rotating speed of 1000-1500r/min for 20-30min, washing with water, and drying to obtain the modified nano silicon dioxide.
Preferably, the grinding agent is prepared by stirring carbon nano tubes and 10-20% of sodium dodecyl sulfate solution according to the weight ratio of 1.
Preferably, the thermal improvement treatment comprises the following specific steps: heating to 450-550 deg.C at a rate of 2-4 deg.C/min, maintaining for 10-20min, and naturally cooling to room temperature.
Preferably, the preparation method of the chitosan modified solution comprises the following steps:
adding 2-3 times of Lewis acid into 10-20% of chitosan solution by mass fraction, then adding 5-10% of phosphoric acid by mass of the chitosan solution, and continuously and fully mixing to obtain the chitosan modified solution.
Preferably, the stirring reaction temperature in the fourth step is 45-55 ℃, the stirring speed is 1000-1500r/min, and the stirring time is 35-45min.
Compared with the prior art, the invention has the following beneficial effects:
according to the molybdenum removal detection method, the tungstate solution is precipitated and vulcanized, the precipitate is firstly carried out, then the bentonite auxiliary modifier is matched with the chitosan modified solution, and the filtrate is further filtered, so that the molybdenum adsorption treatment efficiency is improved.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to specific embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The molybdenum removal detection method for the high-molybdenum tungsten concentrate comprises the following steps of:
the method comprises the following steps: preparing tungsten concentrate into tungstate solution, and then carrying out vulcanization precipitation modification treatment;
step two: preparing an auxiliary modifier for bentonite;
step three: adding bentonite auxiliary modifier into 3-5 times of chitosan modified solution to obtain filtrate treating agent;
step four: stirring the filtrate modified by the precipitation in the step one by using a filtrate treating agent for reaction treatment, and ending the stirring;
step five: and finally filtering, washing and drying the filtrate, and finally detecting the content of molybdenum in the residual filtrate.
The tungstate solution of this example is a sodium tungstate solution with a mass fraction of 10-20%.
The method for modification treatment of sulfide precipitation in this example is: adding hexadecyl trimethyl ammonium bromide accounting for 10-15% of the total amount of the tungstate solution, stirring at the rotating speed of 450-550r/min for 20-30min, and finishing stirring.
The preparation method of the bentonite auxiliary modifier in the embodiment comprises the following steps:
s1: adding bentonite into a hydrochloric acid solution according to the weight ratio of 1;
s2: adding lanthanum sulfate into a sodium alginate solution with the mass fraction of 10-20% which is 3-5 times that of the lanthanum sulfate, and adding modified nano silicon dioxide with the mass fraction of 2-5% of the lanthanum sulfate to obtain a nano silicon dioxide additive;
s3: adding the nano silicon dioxide additive into S1 according to the weight ratio of 1;
s4: and (4) performing thermal improvement treatment on the product of the S3, and finishing the treatment to obtain the bentonite auxiliary modifier.
The mass fraction of the hydrochloric acid solution in the embodiment is 5-10%; the mass fraction of the sodium alginate solution is 10-20%.
The silane coupling agent of the present example is a coupling agent KH560.
The modification method of the modified nano-silica of the embodiment comprises the following steps:
adding 15-20 parts of nano silicon dioxide into 2-5 parts of grinding agent, grinding at the rotating speed of 1000-1500r/min for 20-30min, washing with water, and drying to obtain the modified nano silicon dioxide.
The grinding agent of the embodiment is prepared by stirring carbon nano tubes and 10-20% of sodium dodecyl sulfate solution according to the weight ratio of 1.
The specific steps of the thermal improvement treatment of the embodiment are as follows: heating to 450-550 deg.C at a rate of 2-4 deg.C/min, maintaining for 10-20min, and naturally cooling to room temperature.
The preparation method of the chitosan modification solution of the embodiment comprises the following steps:
adding 2-3 times of Lewis acid into 10-20% of chitosan solution by mass fraction, then adding 5-10% of phosphoric acid by mass of the chitosan solution, and continuously and fully mixing to obtain the chitosan modified solution.
In the fourth step of this embodiment, the temperature of the stirring reaction is 45-55 ℃, the stirring speed is 1000-1500r/min, and the stirring time is 35-45min.
Example 1.
The molybdenum removal detection method for the high-molybdenum tungsten concentrate comprises the following steps of:
the method comprises the following steps: preparing tungsten concentrate into tungstate solution, and then carrying out vulcanization precipitation modification treatment;
step two: preparing an auxiliary modifier for bentonite;
step three: adding bentonite auxiliary modifier into 3-5 times of chitosan modified solution to obtain filtrate treating agent;
step four: stirring the filtrate modified by the precipitation in the step one by using a filtrate treating agent for reaction treatment, and ending the stirring;
step five: and finally, filtering, washing and drying the filtrate, and finally detecting the content of molybdenum in the residual filtrate.
The tungstate solution of this example is a sodium tungstate solution with a mass fraction of 10-20%.
The method for modification treatment of sulfide precipitation in this example is: adding hexadecyl trimethyl ammonium bromide 10-15% of tungstate solution, stirring at 450-550r/min for 20-30min, and stirring.
The preparation method of the bentonite auxiliary modifier in the embodiment comprises the following steps:
s1: adding bentonite into a hydrochloric acid solution according to the weight ratio of 1;
s2: adding lanthanum sulfate into a sodium alginate solution with the mass fraction of 10-20% which is 3-5 times that of the lanthanum sulfate, and adding modified nano silicon dioxide with the mass fraction of 2-5% of the lanthanum sulfate to obtain a nano silicon dioxide additive;
s3: adding the nano silicon dioxide additive into S1 according to the weight ratio of 1;
s4: and (4) performing thermal improvement treatment on the product of the S3, and finishing the treatment to obtain the bentonite auxiliary modifier.
The mass fraction of the hydrochloric acid solution in the embodiment is 5-10%; the mass fraction of the sodium alginate solution is 10-20%.
The silane coupling agent of the present example is a coupling agent KH560.
The modification method of the modified nano-silica of the embodiment comprises the following steps:
adding 15-20 parts of nano silicon dioxide into 2-5 parts of grinding agent, grinding at the rotation speed of 1000-1500r/min for 20-30min, washing with water, and drying to obtain the modified nano silicon dioxide.
The grinding agent of the embodiment is prepared by stirring carbon nano tubes and 10-20% of sodium dodecyl sulfate solution according to the weight ratio of 1.
The specific steps of the thermal improvement treatment of this embodiment are: heating to 450-550 deg.C at a rate of 2-4 deg.C/min, maintaining for 10-20min, and naturally cooling to room temperature.
The preparation method of the chitosan modification solution of the embodiment comprises the following steps:
adding Lewis acid into 2-3 times of 10-20% of chitosan solution by mass fraction, then adding phosphoric acid accounting for 5-10% of the total amount of the chitosan solution, and continuously and fully mixing to obtain the chitosan modified solution.
In the fourth step of this embodiment, the temperature of the stirring reaction is 45-55 ℃, the stirring speed is 1000-1500r/min, and the stirring time is 35-45min.
Example 2.
The molybdenum removal detection method for the high-molybdenum tungsten concentrate comprises the following steps of:
the method comprises the following steps: preparing tungsten concentrate into tungstate solution, and then carrying out vulcanization precipitation modification treatment;
step two: preparing an auxiliary modifier for bentonite;
step three: adding bentonite auxiliary modifier into 3-5 times of chitosan modified solution to obtain filtrate treating agent;
step four: stirring the filtrate modified by the precipitation in the step one by using a filtrate treating agent for reaction treatment, and ending the stirring;
step five: and finally, filtering, washing and drying the filtrate, and finally detecting the content of molybdenum in the residual filtrate.
The tungstate solution of this example is a sodium tungstate solution with a mass fraction of 10-20%.
The method for modification treatment of sulfide precipitation in this example is: adding hexadecyl trimethyl ammonium bromide 10-15% of tungstate solution, stirring at 450-550r/min for 20-30min, and stirring.
The preparation method of the bentonite auxiliary modifier in the embodiment comprises the following steps:
s1: adding bentonite into a hydrochloric acid solution according to the weight ratio of 1;
s2: adding lanthanum sulfate into a sodium alginate solution with the mass fraction of 10-20% which is 3-5 times that of the lanthanum sulfate, and adding modified nano silicon dioxide with the total amount of 2-5% of the lanthanum sulfate to obtain a nano silicon dioxide additive;
s3: adding the nano silicon dioxide additive into S1 according to the weight ratio of 1;
s4: and (4) performing thermal improvement treatment on the product of the S3, and finishing the treatment to obtain the bentonite auxiliary modifier.
The mass fraction of the hydrochloric acid solution in the embodiment is 5-10%; the mass fraction of the sodium alginate solution is 10-20%.
The silane coupling agent of the present example is a coupling agent KH560.
The modification method of the modified nano-silica of the embodiment comprises the following steps:
adding 15-20 parts of nano silicon dioxide into 2-5 parts of grinding agent, grinding at the rotation speed of 1000-1500r/min for 20-30min, washing with water, and drying to obtain the modified nano silicon dioxide.
The grinding agent of the embodiment is prepared by stirring carbon nano tubes and 10-20% of lauryl sodium sulfate solution according to the weight ratio of 1.
The specific steps of the thermal improvement treatment of this embodiment are: heating to 450-550 deg.C at a rate of 2-4 deg.C/min, maintaining for 10-20min, and naturally cooling to room temperature.
The preparation method of the chitosan modification solution of the embodiment comprises the following steps:
adding Lewis acid into 2-3 times of 10-20% of chitosan solution by mass fraction, then adding phosphoric acid accounting for 5-10% of the total amount of the chitosan solution, and continuously and fully mixing to obtain the chitosan modified solution.
In the fourth step of this embodiment, the temperature of the stirring reaction is 45-55 ℃, the stirring speed is 1000-1500r/min, and the stirring time is 35-45min.
Example 3.
The molybdenum removal detection method for the high-molybdenum tungsten concentrate comprises the following steps of:
the method comprises the following steps: preparing tungsten concentrate into tungstate solution, and then carrying out vulcanization precipitation modification treatment;
step two: preparing an auxiliary modifier for bentonite;
step three: adding bentonite auxiliary modifier into 3-5 times of chitosan modified solution to obtain filtrate treating agent;
step four: stirring the filtrate modified by the precipitation in the step one by using a filtrate treating agent for reaction treatment, and ending the stirring;
step five: and finally, filtering, washing and drying the filtrate, and finally detecting the content of molybdenum in the residual filtrate.
The tungstate solution of this example is a sodium tungstate solution with a mass fraction of 10-20%.
The method for modification treatment of sulfide precipitation in this example is: adding hexadecyl trimethyl ammonium bromide 10-15% of tungstate solution, stirring at 450-550r/min for 20-30min, and stirring.
The preparation method of the bentonite auxiliary modifier in the embodiment comprises the following steps:
s1: adding bentonite into a hydrochloric acid solution according to the weight ratio of 1;
s2: adding lanthanum sulfate into a sodium alginate solution with the mass fraction of 10-20% which is 3-5 times that of the lanthanum sulfate, and adding modified nano silicon dioxide with the mass fraction of 2-5% of the lanthanum sulfate to obtain a nano silicon dioxide additive;
s3: adding the nano silicon dioxide additive into S1 according to the weight ratio of 1;
s4: and (4) performing thermal improvement treatment on the product of the S3, and finishing the treatment to obtain the bentonite auxiliary modifier.
The mass fraction of the hydrochloric acid solution in the embodiment is 5-10%; the mass fraction of the sodium alginate solution is 10-20%.
The silane coupling agent of the present example is a coupling agent KH560.
The modification method of the modified nano-silica of the embodiment comprises the following steps:
adding 15-20 parts of nano silicon dioxide into 2-5 parts of grinding agent, grinding at the rotating speed of 1000-1500r/min for 20-30min, washing with water, and drying to obtain the modified nano silicon dioxide.
The grinding agent of the embodiment is prepared by stirring carbon nano tubes and 10-20% of lauryl sodium sulfate solution according to the weight ratio of 1.
The specific steps of the thermal improvement treatment of this embodiment are: heating to 450-550 deg.C at a rate of 2-4 deg.C/min, maintaining for 10-20min, and naturally cooling to room temperature.
The preparation method of the chitosan modification solution of the embodiment comprises the following steps:
adding 2-3 times of Lewis acid into 10-20% of chitosan solution by mass fraction, then adding 5-10% of phosphoric acid by mass of the chitosan solution, and continuously and fully mixing to obtain the chitosan modified solution.
In the fourth step of this embodiment, the temperature of the stirring reaction is 45-55 ℃, the stirring speed is 1000-1500r/min, and the stirring time is 35-45min.
Example 4.
The molybdenum removal detection method for the high-molybdenum tungsten concentrate comprises the following steps of:
the method comprises the following steps: preparing tungsten concentrate into tungstate solution, and then carrying out vulcanization precipitation modification treatment;
step two: preparing an auxiliary modifier for bentonite;
step three: adding bentonite auxiliary modifier into 3-5 times of chitosan modified solution to obtain filtrate treating agent;
step four: stirring the filtrate modified by the precipitation in the step one by using a filtrate treating agent for reaction treatment, and ending the stirring;
step five: and finally, filtering, washing and drying the filtrate, and finally detecting the content of molybdenum in the residual filtrate.
The tungstate solution of this example is a sodium tungstate solution with a mass fraction of 10-20%.
The method for modification treatment of sulfide precipitation in this example is: adding hexadecyl trimethyl ammonium bromide 10-15% of tungstate solution, stirring at 450-550r/min for 20-30min, and stirring.
The preparation method of the bentonite auxiliary modifier in the embodiment comprises the following steps:
s1: adding bentonite into a hydrochloric acid solution according to the weight ratio of 1;
s2: adding lanthanum sulfate into a sodium alginate solution with the mass fraction of 10-20% which is 3-5 times that of the lanthanum sulfate, and adding modified nano silicon dioxide with the total amount of 2-5% of the lanthanum sulfate to obtain a nano silicon dioxide additive;
s3: adding the nano silicon dioxide additive into S1 according to the weight ratio of 1;
s4: and (4) performing thermal improvement treatment on the product of the S3, and finishing the treatment to obtain the bentonite auxiliary modifier.
The mass fraction of the hydrochloric acid solution in the embodiment is 5-10%; the mass fraction of the sodium alginate solution is 10-20%.
The silane coupling agent of the present example is a coupling agent KH560.
The modification method of the modified nano-silica of the embodiment comprises the following steps:
adding 15-20 parts of nano silicon dioxide into 2-5 parts of grinding agent, grinding at the rotating speed of 1000-1500r/min for 20-30min, washing with water, and drying to obtain the modified nano silicon dioxide.
The grinding agent of the embodiment is prepared by stirring carbon nano tubes and 10-20% of lauryl sodium sulfate solution according to the weight ratio of 1.
The specific steps of the thermal improvement treatment of this embodiment are: heating to 450-550 deg.C at a rate of 2-4 deg.C/min, maintaining for 10-20min, and naturally cooling to room temperature.
The preparation method of the chitosan modification solution of the embodiment comprises the following steps:
adding Lewis acid into 2-3 times of 10-20% of chitosan solution by mass fraction, then adding phosphoric acid accounting for 5-10% of the total amount of the chitosan solution, and continuously and fully mixing to obtain the chitosan modified solution.
In the fourth step of this embodiment, the temperature of the stirring reaction is 45-55 ℃, the stirring speed is 1000-1500r/min, and the stirring time is 35-45min.
Comparative example 1.
Unlike example 3, no bentonite co-modifier was added.
Comparative example 2.
The difference from example 3 is that bentonite is used instead of the bentonite auxiliary modifier.
Comparative example 3.
Different from the example 3, no nano silicon dioxide additive is added in the preparation of the bentonite auxiliary modifier.
Comparative example 4.
The difference from example 3 is that the nanosilica additive is replaced by nanosilica.
Comparative example 5.
The difference from the embodiment 3 is that the chitosan modified solution is prepared by adopting chitosan and deionized water according to the weight ratio of 1.
The results of the performance measurements of examples 1 to 4 and comparative examples 1 to 5 are as follows
| Molybdenum removal Rate (%) | |
| Example 1 | 98.5 |
| Example 2 | 98.3 |
| Example 3 | 98.8 |
| Example 4 | 98.3 |
| Comparative example 1 | 68.1 |
| Comparative example 2 | 76.3 |
| Comparative example 3 | 84.7 |
| Comparative example 4 | 87.5 |
| Comparative example 5 | 86.9 |
As is evident from examples 1 to 5 and comparative examples 1 to 5, the product of example 3 of the present invention has an excellent molybdenum removal rate;
it can be seen from comparative examples 1-5 that the product performance is significantly reduced without adding the bentonite auxiliary modifier, and meanwhile, the bentonite auxiliary modifier is replaced by bentonite, the nano-silica additive is not added in the preparation of the bentonite auxiliary modifier, and the nano-silica additive is replaced by nano-silica, so that the performance of the product is deteriorated;
in addition, the product is not treated by the chitosan modifying solution, the performance of the product tends to be deteriorated, and the chitosan modifying solution treatment are cooperated to generate the effect of synergy and enhance the performance improvement effect of the product.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (10)
1. A molybdenum removal detection method for high-molybdenum tungsten concentrate is characterized by comprising the following steps:
the method comprises the following steps: preparing tungsten concentrate into tungstate solution, and then carrying out vulcanization precipitation modification treatment;
step two: preparing an auxiliary modifier for bentonite;
step three: adding bentonite auxiliary modifier into 3-5 times of chitosan modified solution to obtain filtrate treating agent;
step four: stirring the filtrate modified by the precipitation in the step one by adopting a filtrate treating agent for reaction treatment, and ending the stirring;
step five: and finally, filtering, washing and drying the filtrate, and finally detecting the content of molybdenum in the residual filtrate.
2. The molybdenum removal detection method for the high-molybdenum tungsten concentrate according to claim 1, wherein the tungstate solution is a sodium tungstate solution with a mass fraction of 10-20%.
3. The molybdenum removal detection method for the high-molybdenum tungsten concentrate according to claim 1, wherein the method for the modification treatment of the sulfidation precipitation comprises the following steps: adding hexadecyl trimethyl ammonium bromide 10-15% of tungstate solution, stirring at 450-550r/min for 20-30min, and stirring.
4. The molybdenum removal detection method of the high-molybdenum tungsten concentrate according to claim 3, wherein the preparation method of the bentonite auxiliary modifier comprises the following steps:
s1: adding bentonite into a hydrochloric acid solution according to the weight ratio of 1;
s2: adding lanthanum sulfate into a sodium alginate solution with the mass fraction of 10-20% which is 3-5 times that of the lanthanum sulfate, and adding modified nano silicon dioxide with the total amount of 2-5% of the lanthanum sulfate to obtain a nano silicon dioxide additive;
s3: adding the nano silicon dioxide additive into S1 according to the weight ratio of 1;
s4: and (4) performing thermal improvement treatment on the product of the S3, and finishing the treatment to obtain the bentonite auxiliary modifier.
5. The molybdenum removal detection method for the high-molybdenum tungsten concentrate according to claim 4, wherein the mass fraction of the hydrochloric acid solution is 5-10%; the mass fraction of the sodium alginate solution is 10-20%.
6. The molybdenum removal detection method of the high-molybdenum tungsten concentrate according to claim 4, wherein the silane coupling agent is a coupling agent KH560.
7. The molybdenum removal detection method for the high-molybdenum tungsten concentrate according to claim 4, wherein the modification method of the modified nano-silica comprises the following steps:
adding 15-20 parts of nano silicon dioxide into 2-5 parts of grinding agent, grinding at the rotating speed of 1000-1500r/min for 20-30min, washing with water, and drying to obtain modified nano silicon dioxide;
the grinding agent is prepared by stirring carbon nano tubes and 10-20% of lauryl sodium sulfate solution according to the weight ratio of 1.
8. The molybdenum removal detection method for the high-molybdenum tungsten concentrate according to claim 4, characterized in that the thermal improvement treatment comprises the following specific steps: heating to 450-550 deg.C at a rate of 2-4 deg.C/min, maintaining for 10-20min, and naturally cooling to room temperature.
9. The molybdenum removal detection method for the high-molybdenum tungsten concentrate according to claim 1, characterized in that the preparation method of the chitosan modification solution comprises the following steps:
adding Lewis acid into 2-3 times of 10-20% of chitosan solution by mass fraction, then adding phosphoric acid accounting for 5-10% of the total amount of the chitosan solution, and continuously and fully mixing to obtain the chitosan modified solution.
10. The molybdenum removal detection method for the high-molybdenum tungsten concentrate according to claim 1, wherein the stirring reaction temperature in the fourth step is 45-55 ℃, the stirring rotation speed is 1000-1500r/min, and the stirring time is 35-45min.
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| CN111154991A (en) * | 2020-01-19 | 2020-05-15 | 北京工业大学 | Method for separating tungsten and molybdenum from tungsten molybdate solution |
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| CN101220418A (en) * | 2008-01-29 | 2008-07-16 | 辽宁大学 | Method for separating molybdenum, rhenium from molybdenum mineral |
| CN101531735A (en) * | 2009-04-17 | 2009-09-16 | 中南大学 | Modified resin used for removing tungsten deeply in molybdate solution and preparation thereof |
| CN101880780A (en) * | 2010-06-04 | 2010-11-10 | 中南大学 | Method for separating and extracting tungsten-molybdenum from mixed solution of tungstate-molybdate |
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