CN108452765A - The method of porous silicon adsorption material and porous silicon adsorption material are prepared using low-grade diatomite - Google Patents
The method of porous silicon adsorption material and porous silicon adsorption material are prepared using low-grade diatomite Download PDFInfo
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- CN108452765A CN108452765A CN201810135746.1A CN201810135746A CN108452765A CN 108452765 A CN108452765 A CN 108452765A CN 201810135746 A CN201810135746 A CN 201810135746A CN 108452765 A CN108452765 A CN 108452765A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/14—Diatomaceous earth
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28061—Surface area, e.g. B.E.T specific surface area being in the range 100-500 m2/g
Abstract
The method of porous silicon adsorption material is prepared the invention discloses a kind of using low-grade diatomite and porous silicon adsorption material, method include the following steps:1) roasting diatomite is prepared;2) alkali soaks desiliconization;3) it is filtered, washed;4) active lime breast is prepared;5) porous silicon adsorption material is made.The raw material sources of the present invention are abundant extensive, and low raw-material cost prepares sorbing material by cheap lime stone and low-grade diatomite, and technology of preparing is simple, and technological process is short, and comprehensive energy consumption is relatively low, and production cost is low;The loose bulk density of the porous silicon adsorption material prepared using the method for the present invention is 0.20~0.32g/m3, specific surface area is 130~160m2/ g, PARA FORMALDEHYDE PRILLS(91,95), benzene, SO2And volatile heavy metal has good absorption property.
Description
Technical field:
The present invention relates to a kind of method preparing porous silicon adsorption material and porous silicon adsorption materials, more particularly to one kind
The method of porous silicon adsorption material and porous silicon adsorption material are prepared using low-grade diatomite.
Background technology:
Diatomite (Diatomite) is a kind of biogenic siliceous sedimentary rock, and main chemical compositions are SiO2, usually
SiO2Content higher show that diatomaceous precision grade is higher.The diatomite ore reserve in China is compared with horn of plenty, still, big portion
Divide diatomite ore product position relatively low, for dioxide-containing silica mostly 50% or so, low-grade diatomite accounts for overall reserves
70% or so.Since enterprise product is single, the products such as filter aid, catalyst are relatively high to the requirement of diatomaceous credit rating, make
At level-one diatomite in diatomite recovery process, is only exploited, a large amount of low-grade diatomite abandoned does not obtain profit appropriate
With;Meanwhile in exploitation process from now on, the cost of winning and difficulty of diatomite ore increase.
Currently, low-grade diatomite (SiO2≤ 80%) it mainly for the production of thermal insulation material and light-weight building material, adds
It is worth relatively low.Therefore, how to realize that low-grade diatomaceous recycling, high-valued large utilize are asked as in the urgent need to address
Topic.
Chinese invention patent (CN103253951A) reports a kind of preparation of low-grade diatomite-based composite porous material
Method passes through dispensing, ball milling, granulation, aging, molding, drying using low-grade diatomite, sugared filter mud and industrial residue as raw material
Product is made with sintering, but this method technological process is longer, sintering process energy consumption is higher, for added value in terms of decorative building material
It is relatively low;Chinese invention patent CN102600818A reports a kind of calcium oxide-based sorbing material of tripolite loading, is to utilize leaching
The stain precipitation method load to calcium oxide in diatomite matrix, but this method the defects of there are complex process, meanwhile, the adsorption material
Material is just for CO2Absorption, it is insufficient to volatile organic matter absorption property;Chinese invention patent CNIO2641720A is reported
A kind of preparation method of modification infusorial earth composite adsorbing material is by diatomite and to be dissolved in ferric salt solution first
Chitosan is uniformly mixed;Then it precipitated after addition ethyl alcohol, be filtered, washed drying;Desciccate is finally placed in the second of glutaraldehyde
Reaction is crosslinked in alcoholic solution, composite adsorbing material is obtained after precipitation is dry, but this method technology of preparing is complicated, technique stream
Journey is longer, and production cost is higher.
Invention content:
The purpose of the present invention is to provide a kind of low cost, the low-grade diatomite of utilization that flow is short, technically simple to prepare
The method and PARA FORMALDEHYDE PRILLS(91,95) of porous silicon adsorption material, benzene, SO2And volatile heavy metal has the porous of good absorption property
Silicon adsorption material.
The purpose of the present invention is implemented by following technical solution:It is a kind of to prepare porous silicon adsorption material using low-grade diatomite
Method comprising following steps:1) roasting diatomite is prepared;2) alkali soaks desiliconization;3) it is filtered, washed;4) high activity stone is prepared
Grey breast;5) porous silicon adsorption material is made;Wherein,
1) roasting diatomite is prepared:By low-grade diatomite crushing and grinding, 1-3h is roasted under the conditions of 200~300 DEG C, is gone
It except organic matter therein, is then sieved, obtains the roasting diatomite that granularity is more than 325 mesh;Removal organic matter is conducive to alkali
The progress for soaking desilication reaction, avoids enter into desiliconization liquid, while can improve the purity of porous adsorbing material, reduces therein miscellaneous
Matter content.
2) alkali soaks desiliconization:The roasting diatomite and certain density sodium hydroxide solution are mixed, alkali leaching is carried out
Desilication reaction obtains suspension slurry system;
3) it is filtered, washed:The suspension slurry system is filtered isolated filter cake and filtrate, using process water pair
The filter cake is washed, and sieving removing suspended impurity, obtains desiliconization solution after the washings after washing are mixed with filtrate, described
Filter cake obtains desiliconization slag after repeatedly washing;
4) active lime breast is prepared:Quick lime plus water are digested to obtain active lime breast;Active lime breast
Refer to the calcium oxide content height wherein dissolved, without inactive calcium oxide impurity.
5) porous silicon adsorption material is made:Desiliconization solution obtained by milk of lime obtained by step 4) and step 3) is mixed,
Reaction after the completion of be filtered, washed, isolated filtering filter cake and recycle sodium hydroxide solution;The filtering filter cake drying, powder
Mill obtains porous silicon adsorption material.
Specifically, SiO in low-grade diatomite in the step 1)2Mass percentage be less than 80%.
Specifically, in the step 2), the mass concentration of the sodium hydroxide solution is 5~30%.
Specifically, in the step 2), the SiO in low-grade diatomite2Molal weight ratio with sodium hydroxide is 0.5:1
~1.5.
Specifically, in the step 2), the desilication reaction temperature of low-grade diatomite and sodium hydroxide solution is 80~220
DEG C, the desilication reaction time is 0.5~3 hour.
Specifically, in the step 4), quick lime is calcined after limestone calcination or carbide slag pickling impurity removal;Raw stone
The mass ratio of ash and water is 1:3~8, the temperature of water is 60~95 DEG C.
Specifically, in the step 5), Ca (OH) in milk of lime2With SiO in desiliconization solution2Stoichiometric ratio be 0.6~
1:1, reaction temperature is 90~130 DEG C, and the reaction time is 0.5~2.5 hour.
Specifically, in the step 5), the drying temperature of the filtering filter cake is 150~400 DEG C, drying time 0.5
~8 hours.
Specifically, returning to cycle in the step 1) in the step 5), after the recycling sodium hydroxide solution concentration makes
With the mass concentration of sodium hydroxide solution is 10~12% after recycling concentration.
The porous silicon prepared using a kind of method preparing porous silicon adsorption material using low-grade diatomite is inhaled
Enclosure material.
Advantages of the present invention:(1) raw material sources of the invention are abundant extensive, and low raw-material cost passes through cheap lime
Stone and low-grade diatomite prepare sorbing material, and technology of preparing is simple, and technological process is short, and comprehensive energy consumption is relatively low, production cost
It is low;(2) sorbing material product large specific surface area of the present invention, the chemical composition and stable in physicochemical property of product are organic to volatility
The absorbent properties of object are excellent, and added value of product is high;(3) in the present invention, sodium hydroxide can recycle, the recycling of sodium hydroxide
Rate further reduced the cost of material of sorbing material up to 70~80%;(4) porous silicon adsorption material prepared by the method for the present invention
Loose bulk density be 0.20~0.32g/m3, specific surface area is 130~160m2/ g, PARA FORMALDEHYDE PRILLS(91,95), benzene, SO2And volatility
Heavy metal has good absorption property.
Description of the drawings:
Fig. 1 is embodiment 1-3 process flow charts.
Specific implementation mode:
Embodiment 1:A method of preparing porous silicon adsorption material using low-grade diatomite comprising following steps:
1) roasting diatomite is prepared;2) alkali soaks desiliconization;3) it is filtered, washed;4) active lime breast is prepared;5) porous silicon adsorption material is made
Material;Wherein,
1) roasting diatomite is prepared:By SiO2Mass percentage be 68% low-grade diatomite 10Kg be crushed powder
Mill, roasts 1.5h under the conditions of 250 DEG C, removes organic matter therein, then sieved, and obtains the roasting that granularity is more than 325 mesh
Burn diatomite;.
2) alkali soaks desiliconization:By it is described roasting diatomite and mass concentration be 20% sodium hydroxide solution in reaction kettle,
Mechanical agitation mixes, and carries out alkali and soaks desilication reaction, desilication reaction temperature is 80 DEG C, and the desilication reaction time is 3 hours, is suspended
Slurry system;Wherein, the SiO in low-grade diatomite2Molal weight ratio with sodium hydroxide is 0.5:1.2;
3) it is filtered, washed:The suspension slurry system is filtered isolated filter cake and filter by vacuum filter
Liquid washs the filter cake using process water, and sieving removing suspended impurity, obtains after the washings after washing are mixed with filtrate
To desiliconization solution, the filter cake obtains desiliconization slag after repeatedly washing;
4) active lime breast is prepared:Quick lime plus water are digested to obtain active lime breast;Quick lime comes from stone
It is calcined after lime stone calcining or carbide slag pickling impurity removal;The mass ratio of quick lime and water is 1:3, the temperature of water is 65 DEG C;
5) porous silicon adsorption material is made:Desiliconization solution obtained by milk of lime obtained by step 4) and step 3) is placed in reaction kettle
Middle mixing, stir speed (S.S.) 150r/min, Ca (OH) in milk of lime2With SiO in desiliconization solution2Stoichiometric ratio be
0.6:1, reaction temperature be 95 DEG C, reaction time 70min, reaction after the completion of be filtered, washed, isolated filtering filter cake and time
Receive sodium hydroxide solution;The filtering filter cake drying, grinding obtain porous silicon adsorption material, the drying temperature of the filtering filter cake
Degree is 300 DEG C, and drying time is 5 hours;A small amount of sodium hydroxide is supplemented after recycling sodium hydroxide solution concentration, described in return
It is recycled in step 1), the mass concentration of sodium hydroxide solution is 10% after recycling concentration.
Utilize a kind of above-mentioned porous silicon absorption prepared by the method for preparing porous silicon adsorption material using low-grade diatomite
Material, physicochemical property are:Granularity is 3.5 μm;Bulk density is 0.32g/cm3;Specific surface area 143m2/g。
Embodiment 2:A method of preparing porous silicon adsorption material using low-grade diatomite comprising following steps:
1) roasting diatomite is prepared;2) alkali soaks desiliconization;3) it is filtered, washed;4) active lime breast is prepared;5) porous silicon adsorption material is made
Material;Wherein,
1) roasting diatomite is prepared:By SiO2Content is the low-grade diatomite 10Kg crushing and grindings of 72%wt, at 300 DEG C
Under the conditions of roast 3h, remove organic matter therein, then sieved, obtain granularity be more than 325 mesh roasting diatomite;
2) alkali soaks desiliconization:The sodium hydroxide solution that the roasting diatomite and mass concentration are 5% is uniformly mixed postposition
In reaction kettle, mechanical agitation carries out alkali and soaks desilication reaction, and continuous mechanical agitation during desilication reaction keeps desiliconization anti-
That answers is uniform.Desilication reaction temperature is 110 DEG C, and the desilication reaction time is 3 hours, obtains suspension slurry system;Wherein, low-grade
SiO in diatomite2Molal weight ratio with sodium hydroxide is 0.5:1;
3) it is filtered, washed:The suspension slurry system is filtered isolated filter cake and filter by vacuum filter
Liquid washs the filter cake using process water, and sieving removing suspended impurity, obtains after the washings after washing are mixed with filtrate
To desiliconization solution, the filter cake obtains desiliconization slag after repeatedly washing;
4) active lime breast is prepared:Quick lime plus water are digested to obtain active lime breast;Quick lime comes from stone
It is calcined after lime stone calcining or carbide slag pickling impurity removal;The mass ratio of quick lime and water is 1:5, the temperature of water is 95 DEG C;
5) porous silicon adsorption material is made:Desiliconization solution obtained by milk of lime obtained by step 4) and step 3) is placed in reaction kettle
Middle mixing, stir speed (S.S.) 100r/min.Ca (OH) in milk of lime2With SiO in desiliconization solution2Stoichiometric ratio be 1:
1, reaction temperature is 105 DEG C, reaction time 30min, is filtered, washed after the completion of reaction, isolated filtering filter cake and recycling
Sodium hydroxide solution;The filtering filter cake drying, grinding obtain porous silicon adsorption material, the drying temperature of the filtering filter cake
It is 400 DEG C, drying time 30min;A small amount of sodium hydroxide, which is supplemented, after the recycling sodium hydroxide solution concentration returns to the step
Rapid 1) middle recycling, the mass concentration of sodium hydroxide solution is 11% after recycling concentration.
Utilize a kind of above-mentioned porous silicon absorption prepared by the method for preparing porous silicon adsorption material using low-grade diatomite
Material, physicochemical property are:Granularity is 2.8 μm;Bulk density is 0.20g/cm3;Specific surface area 156m2/g。
Embodiment 3:A method of preparing porous silicon adsorption material using low-grade diatomite comprising following steps:
1) roasting diatomite is prepared;2) alkali soaks desiliconization;3) it is filtered, washed;4) active lime breast is prepared;5) porous silicon adsorption material is made
Material;Wherein,
1) roasting diatomite is prepared:By SiO2Content is the low-grade diatomite 10Kg crushing and grindings of 70%wt, at 200 DEG C
Under the conditions of roast 1h, remove organic matter therein, then sieved, obtain granularity be more than 325 mesh roasting diatomite;
2) alkali soaks desiliconization:The sodium hydroxide solution that the roasting diatomite and mass concentration are 30% is uniformly mixed postposition
In reaction kettle, mechanical agitation carries out alkali and soaks desilication reaction, and continuous mechanical agitation during desilication reaction keeps desiliconization anti-
That answers is uniform.Desilication reaction temperature is 220 DEG C, and the desilication reaction time is 0.5 hour, obtains suspension slurry system;Wherein, low product
SiO in the diatomite of position2Molal weight ratio with sodium hydroxide is 0.5:1.5;
3) it is filtered, washed:The suspension slurry system is filtered isolated filter cake and filter by vacuum filter
Liquid washs the filter cake using process water, and sieving removing suspended impurity, obtains after the washings after washing are mixed with filtrate
To desiliconization solution, the filter cake obtains desiliconization slag after repeatedly washing;
4) active lime breast is prepared:Quick lime plus water are digested to obtain active lime breast;Quick lime comes from stone
It is calcined after lime stone calcining or carbide slag pickling impurity removal;The mass ratio of quick lime and water is 1:8, the temperature of water is 60 DEG C;
5) porous silicon adsorption material is made:Desiliconization solution obtained by milk of lime obtained by step 4) and step 3) is placed in reaction kettle
Middle mixing, stir speed (S.S.) 100r/min.Ca (OH) in milk of lime2With SiO in desiliconization solution2Stoichiometric ratio be
0.8:1, reaction temperature be 90 DEG C, the reaction time be 2.5 hours, reaction after the completion of be filtered, washed, isolated filtering filter cake and
Recycle sodium hydroxide solution;The filtering filter cake drying, grinding obtain porous silicon adsorption material, the drying of the filtering filter cake
Temperature is 150 DEG C, and drying time is 8 hours;A small amount of sodium hydroxide, which is supplemented, after the recycling sodium hydroxide solution concentration returns to institute
It states in step 1) and recycles, the mass concentration of sodium hydroxide solution is 12% after recycling concentration.
Utilize a kind of above-mentioned porous silicon absorption prepared by the method for preparing porous silicon adsorption material using low-grade diatomite
Material, physicochemical property are:Granularity is 2.8 μm;Bulk density is 0.28g/cm3;Specific surface area 160m2/g。
Porous silicon adsorption material made from embodiment 1-3 is as shown in the table to the absorbent properties of volatile organic gases:
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.
Claims (10)
1. a kind of method preparing porous silicon adsorption material using low-grade diatomite, which is characterized in that it includes the following steps:
1) roasting diatomite is prepared;2) alkali soaks desiliconization;3) it is filtered, washed;4) active lime breast is prepared;5) porous silicon adsorption material is made
Material;Wherein,
1) roasting diatomite is prepared:By low-grade diatomite crushing and grinding, 1-3h is roasted under the conditions of 200~300 DEG C, removes it
In organic matter, then sieved, obtain granularity be more than 325 mesh roasting diatomite;
2) alkali soaks desiliconization:The roasting diatomite and certain density sodium hydroxide solution are mixed, alkali is carried out and soaks desiliconization
Reaction, obtains suspension slurry system;
3) it is filtered, washed:The suspension slurry system is filtered isolated filter cake and filtrate, the filter cake is washed
It washs, sieving removing suspended impurity after the washings after washing are mixed with filtrate obtains desiliconization solution, and the filter cake is through repeatedly washing
After obtain desiliconization slag;
4) active lime breast is prepared:Quick lime plus water are digested to obtain active lime breast;
5) porous silicon adsorption material is made:Desiliconization solution obtained by milk of lime obtained by step 4) and step 3) is mixed, reaction
Be filtered, washed after the completion, isolated filtering filter cake and recycling sodium hydroxide solution;The filtering filter cake drying, grinding obtain
To porous silicon adsorption material.
2. a kind of method preparing porous silicon adsorption material using low-grade diatomite according to claim 1, feature
It is, SiO in the low-grade diatomite in the step 1)2Mass percentage be less than 80%.
3. a kind of method preparing porous silicon adsorption material using low-grade diatomite according to claim 1, feature
It is, in the step 2), the mass concentration of the sodium hydroxide solution is 5~30%.
4. a kind of method preparing porous silicon adsorption material using low-grade diatomite according to claim 1, feature
It is, in the step 2), the SiO in low-grade diatomite2Molal weight ratio with sodium hydroxide is 0.5:1~1.5.
5. a kind of method preparing porous silicon adsorption material using low-grade diatomite according to claim 1, feature
It is, in the step 2), the desilication reaction temperature of low-grade diatomite and sodium hydroxide solution is 80~220 DEG C, and desiliconization is anti-
It is 0.5~3 hour between seasonable.
6. a kind of method preparing porous silicon adsorption material using low-grade diatomite according to claim 1, feature
It is, in the step 4), the mass ratio of quick lime and water is 1:3~8, the temperature of water is 60~95 DEG C.
7. a kind of method preparing porous silicon adsorption material using low-grade diatomite according to claim 1, feature
It is, in the step 5), Ca (OH) in milk of lime2With SiO in desiliconization solution2Stoichiometric ratio be 0.6~1:1, reaction temperature
Degree for 90~
130 DEG C, the reaction time is 0.5~2.5 hour.
8. a kind of method preparing porous silicon adsorption material using low-grade diatomite according to claim 1, feature
It is, in the step 5), the drying temperature of the filtering filter cake is 150~400 DEG C, and drying time is 0.5~8 hour.
9. a kind of method preparing porous silicon adsorption material using low-grade diatomite according to claim 1, feature
It is, in the step 5), returns in the step 1) and recycle after the recycling sodium hydroxide solution concentration, recycling concentration
The mass concentration of sodium hydroxide solution is 10~12% afterwards.
10. described a kind of preparing porous silicon adsorption material using low-grade diatomite using described in any one of claim 1-9
Porous silicon adsorption material prepared by method.
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CN109939646A (en) * | 2019-03-01 | 2019-06-28 | 牟丽慰 | A kind of preparation method of super-cell |
CN112028709A (en) * | 2020-08-06 | 2020-12-04 | 内蒙古工业大学 | Application of active silicon material in preparation of water-retention slow-release microbial fertilizer |
CN112265180A (en) * | 2020-09-30 | 2021-01-26 | 方少山 | Universal white master batch and preparation method thereof |
CN112569965A (en) * | 2020-12-23 | 2021-03-30 | 内蒙古工业大学 | Double-transition metal hierarchical pore catalyst and preparation method and application thereof |
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CN112265180A (en) * | 2020-09-30 | 2021-01-26 | 方少山 | Universal white master batch and preparation method thereof |
CN112569965A (en) * | 2020-12-23 | 2021-03-30 | 内蒙古工业大学 | Double-transition metal hierarchical pore catalyst and preparation method and application thereof |
CN112569965B (en) * | 2020-12-23 | 2022-09-09 | 内蒙古工业大学 | Double-transition metal hierarchical pore catalyst and preparation method and application thereof |
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CN114394865A (en) * | 2022-02-08 | 2022-04-26 | 重庆大学 | Diatomite-based slow-release compound fertilizer and granulation mode |
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