CN110395753A - A kind of preparation method of epigranular high stable houghite - Google Patents
A kind of preparation method of epigranular high stable houghite Download PDFInfo
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- CN110395753A CN110395753A CN201910606824.6A CN201910606824A CN110395753A CN 110395753 A CN110395753 A CN 110395753A CN 201910606824 A CN201910606824 A CN 201910606824A CN 110395753 A CN110395753 A CN 110395753A
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- houghite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/78—Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen
- C01F7/784—Layered double hydroxide, e.g. comprising nitrate, sulfate or carbonate ions as intercalating anions
- C01F7/785—Hydrotalcite
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a kind of preparation methods of epigranular high stable houghite, belong to metal oxide preparation technical field.The present invention mixes bean dregs with starch, the protein in bean dregs, plant fiber hydrolysis is set to generate the ingredients such as amino acid, cellulose by high-temperature high-voltage reaction, cellulose, the hydroxyl group oxidation in plant fiber is set to generate carboxylic group using sulfuric acid and potassium permanganate, esterification occurs with ethylene glycol again to condense part ester type compound in fiber surface, each ingredient in absorption houghite is bonded using plant fiber, it avoids making houghite product there is a situation where size distribution unevenness, improves the compatibility of houghite and other materials；The organic principles such as cellulose, saccharide compound are extracted in present invention hydrolysis from bean dregs and starch, bonding suction-operated is formed to ingredients other in houghite using each organic matter, mixed crystallization is nucleated at high temperature, is improved the structural strength of houghite, is enhanced the durability and stability of houghite.
Description
Technical field
The invention discloses a kind of preparation methods of epigranular high stable houghite, belong to metal oxide preparation skill
Art field.
Background technique
Houghite (HTlc) is also referred to as layered di-hydroxyl composite metal oxidate, is a kind of anionic clay.Structure
Similar to shepardite.LDHs has layer structure, the adjustable denaturation of laminate element and the interchangeability of interlayer anion.It is this
The special nature showed on chemistry and structure assigns its a variety of property, such as thermal stability, alkalinity and memory effectiveness
Deng, and have application prospect in various aspects such as heat stabilizer, fire retardant, new catalysts.
Recent years, HTlc caused the broad interest of people, because the structure and performance of HTlc determine that it is raw in industry
Many of production technology potential application, such as anionite, sensor, optical bodies, ceramic forerunner, adsorbent, ion
Conductor, catalyst and catalyst precursor etc..
That most commonly seen is MgAl (OH) pqH2O.Houghite can develop multiple functions material, be widely used as selectivity
Infrared absorption, ultraviolet-resistant, the nontoxic fire retardant of high suppression cigarette and organic articles heat stabilizer, environmentally friendly catalyst, novel suction
Enclosure material, multifunctional carrier, ion exchange material, Medicine material, antibacterial and mouldproof material, new construction performance function material
Prepare precursor etc., become the hot spot that developed country in recent years competitively researches and develops.
For houghite, most commonly seen preparation method is liquid-phase precipitation method in the prior art, usually in intermittent stirring
It is carried out in tank reactor.Wang Rongtao etc. (functional material, 2009,40 (12), 2119-2122) is prepared for using liquid-phase precipitation method
Nano-sized carbon acid group type magnalium hydrotalcite.Xie Xianmei etc. (chemistry of fuel journal, 2003,31 (6), 620-623) uses liquid-phase precipitation
Method is prepared for NiMgAl ternary hydrotalcite.However, due to mixing efficiency microcosmic in stirred-tank reactor is poor, Temperature Distribution not
, the nucleation rate of different location with growth rate differs larger in kettle, so that there are Granularity Distributions for conventional production methods
Between uneven, batch the problems such as poor repeatability.It is past for the uniform mixing for reaching microscopic units for batch stirred tank reactor
Toward using high energy consumption as cost, it is unfavorable for industrial production.For make via liquid-phase precipitation method prepare nano hydrotalcite homogeneous grain diameter,
Performance is stablized, and can strengthen microcosmic mixing there is an urgent need to one kind and conduct heat and have the technology of low energy consumption.
Micro- Chemical Engineering Technology is the Environment Science field of the multi-crossed disciplines risen early 1990s.The technology it is main
Feature is to realize various unit operations and reaction process in tens of microchannels to hundreds of microns magnitude using characteristic size.Due to
Channel size is substantially reduced, and Mass and heat transfer process is significantly strengthened, can increase substantially in reaction process the utilization efficiency of the energy and
The production capacity of unit volume realizes chemical process reinforcing, micromation and greenization.In recent years, it is prepared using micro- Chemical Engineering Technology
Nano material has caused the extensive concern of academia and industry.However, carrying out houghite preparation in micro passage reaction
Report it is less.Abello etc. discloses a kind of method that small volume reactor prepares hydrotalcite, and the reactor outer wall is equipped with solid
Ledger-plate, bottom are equipped with rotor, and revolving speed is up to 24000rpm.High-speed rotating liquid is sheared come strong by outer wall blade when reaction
Change mixing, but there are agglomeration traits for gained hydrotalcite product.Additionally due to rotor high speed rotation, energy consumption is high, is unfavorable for industrial life
It produces.
Therefore, the houghite for inventing a kind of even particle size distribution is necessary to metal oxide preparation technical field
's.
Summary of the invention
The technical problems to be solved by the invention: for mixing effect microcosmic in reactor in current houghite preparation process
Rate is poor, temperature distributing disproportionation, and the nucleation rate of different location differs the larger houghite for leading to preparation with growth rate in kettle
The defect of poor repeatability and houghite durability difference between Granularity Distribution unevenness, batch, it is equal to provide a kind of granularity
The preparation method of even high stable houghite.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
A kind of epigranular high stable houghite the preparation method comprises the following steps:
(1) by modifiers dispersants, aluminium oxide, silica, magnesia investment blender, in temperature be 45~55 DEG C and stirring turns
Speed is that the revolving speed of 500~600r/min is stirred 50~60min, filter residue is obtained by filtration after stirring, wash with distilled water filter residue 3
~5 times up to hybrid solid product；
(2) by hybrid solid product and distilled water investment reaction kettle, the hydrogen that mass fraction is 10~12% is added dropwise into reaction kettle
Sodium hydroxide solution adjusts pH value to 11~12, and 30~40min is mixed with the revolving speed of 300~400r/min with blender, stirs
Reactor temperature is increased to 120~130 DEG C of 40~50min of isothermal reaction after mixing, filter residue is obtained by filtration after reaction, with distillation
Water cleans filter residue 3~5 times, puts into baking oven, ground 50 mesh of dry 3~4h discharging under conditions of temperature is 110~120 DEG C
It sieves up to epigranular high stable houghite；
The preparation of mixed serum are as follows:
(1) bean dregs and starch are put into vacuum oven, in the item that temperature is 50~60 DEG C and vacuum degree is 100~200Pa
Dry 3~4h obtains dried material under part, is in mass ratio 1:10 investment high-temperature high-pressure reaction kettle by dried material and distilled water
In, air pressure in reaction kettle is increased to 0.5~0.7MPa, temperature is increased to 115~125 DEG C, and constant temperature and pressure reacts 40~50min
Reaction mixture is made；
(2) hydrochloric acid that reaction mixture and mass fraction are 10~15% is put into beaker, placing the beaker bath temperature is 40
In~50 DEG C of water-bath, 40~50min is mixed with the revolving speed of 300~400r/min with blender, acidic mixed is made
Aluminum chloride powder is added into beaker for liquid, continues 30~40min of stirring and mixed serum is made；
The preparation of modifiers dispersants are as follows:
(1) potassium permanganate powder is added into beaker, places the beaker in sonic oscillation instrument, in the item that frequency is 36~40kHz
Oxidation liquid is made in 30~40min of oscillation mixing under part, the sulfuric acid solution for being 15~20% by oxidation liquid and mass fraction
It puts into be uniformly mixed in three-necked flask and be made to reaction solution；
(2) ethylene glycol solution for being 30~35% to the mass fraction of reaction solution quality 20~30% is added into three-necked flask, it will
Three-necked flask is placed in resistance heating set, and temperature in heating mantle is increased to 60~70 DEG C, with blender with 500 under constant temperature
The revolving speed of~550r/min stirs 2~3h, puts into Rotary Evaporators after pH value to neutrality is adjusted after stirring, is 250 in revolving speed
Modifiers dispersants are made in 60~80min of concentration under conditions of~300r/min and temperature are 50~70 DEG C.
Preferably according to parts by weight, the modifiers dispersants are 20~22 parts, aluminium oxide is 2~3 parts, silica is
4~6 parts, magnesia be 4~5 parts.
The mass ratio of the hybrid solid product and distilled water is 1:10.
The mass ratio of bean dregs described in the specific preparation step (1) of mixed serum and starch is 5:1.
The hydrochloric acid that reaction mixture described in the specific preparation step (1) of mixed serum and mass fraction are 10~15%
Mass ratio be 5:1.
The quality for the aluminum chloride powder being added described in the specific preparation step (1) of mixed serum into beaker is acidity
The 6~8% of mixed liquor quality.
The quality for the potassium permanganate powder being added described in the specific preparation step (1) of modifiers dispersants into beaker is
The 6~10% of mixed serum quality.
The sulphur that oxidation liquid described in the specific preparation step (1) of modifiers dispersants and mass fraction are 15~20%
The mass ratio of acid solution is 5:1.
The mass fraction being added described in the specific preparation step (1) of modifiers dispersants into three-necked flask be 30~
The quality of 35% ethylene glycol solution is 20~30% to reaction solution quality.
The method have the benefit that:
(1) present invention mixes progress high-temperature high-voltage reaction and is made and react after dry first by bean dregs and starch combination drying with water
Mixed liquor, then reaction mixture is reacted with mixed in hydrochloric acid, aluminium chloride is added after reaction, mixed serum is made, then thereto
Potassium permanganate is added and sulfuric acid is mixed to prepare to reaction solution, will be then mixed to which ethylene glycol is added in reaction solution, after stirring
Modifiers dispersants are made in concentration and evaporation, then the material mixings such as modifiers dispersants and aluminium chloride, silica are stirred, and filter after stirring
Hybrid solid product is obtained, hybrid solid product is mixed with water finally, lye pyroreaction is added dropwise again, filtering drying after reaction
Up to epigranular high stable houghite, bean dregs are mixed with starch, are made in bean dregs by high-temperature high-voltage reaction by the present invention
Protein, plant fiber hydrolysis generate the ingredients such as amino acid, cellulose, keep cellulose, plant fine using sulfuric acid and potassium permanganate
Hydroxyl group oxidation in dimension generates carboxylic group, then esterification occurs to condense part ester in fiber surface with ethylene glycol
Class compound, using plant fiber bond absorption houghite in each ingredient, be conducive to houghite in nucleation and crystallization, respectively at
Divide and is bonded in fiber surface, it is evenly dispersed using cellulose components, to avoid making houghite product that size distribution occur not
Equal situation, while each oxide components in cellulose bonding absorption hydrotalcite, can utilize the ester type compound covering portion on surface layer
It is divided into point, is inhaled so that houghite and other materials be enable to form covalent bond, intermolecular force and other chemical bond energys
It is attached, improve the compatibility of houghite and other materials；
(2) organic principles such as cellulose, saccharide compound are extracted in present invention hydrolysis from bean dregs and starch, utilize each organic matter pair
Other ingredients form bonding suction-operated in houghite, and mixed crystallization is nucleated at high temperature, are further formed and are closely inhaled
Attached effect, so that the degree of absorption in houghite microstructure between each ingredient is improved, it is strong with the structure for improving houghite
Degree, enhances the durability and stability of houghite, has broad application prospects.
Specific embodiment
It is in mass ratio in 5:1 investment vacuum oven by bean dregs and starch, in temperature be 50~60 DEG C and vacuum degree is
Dry 3~4h obtains dried material under conditions of 100~200Pa, is in mass ratio 1:10 investment by dried material and distilled water
In high-temperature high-pressure reaction kettle, air pressure in reaction kettle is increased to 0.5~0.7MPa, temperature is increased to 115~125 DEG C, and constant temperature is permanent
Reaction mixture is made in 40~50min of pressure reaction；The hydrochloric acid that above-mentioned reaction mixture and mass fraction are 10~15% is pressed into quality
Than being put into beaker for 5:1, place the beaker in the water-bath that bath temperature is 40~50 DEG C, with blender with 300~400r/
The revolving speed of min is mixed 40~50min and acid mixed solution is made, and the chlorine of acid mixed solution quality 6~8% is added into beaker
Change aluminium powder, continues 30~40min of stirring and mixed serum is made；6~10% Gao Meng of mixed serum quality is added into above-mentioned beaker
Sour potassium powder, places the beaker in sonic oscillation instrument, oscillation mixing 30~40min system under conditions of frequency is 36~40kHz
Oxidation liquid is obtained, is in mass ratio that 5:1 puts into three mouthfuls of burnings by the sulfuric acid solution that oxidation liquid and mass fraction are 15~20%
It is uniformly mixed and is made to reaction solution in bottle；It is added into above-mentioned three-necked flask and is to the mass fraction of reaction solution quality 20~30%
Three-necked flask is placed in resistance heating set, temperature in heating mantle is increased to 60~70 DEG C by 30~35% ethylene glycol solution,
2~3h is stirred with the revolving speed of 500~550r/min with blender under constant temperature, puts into rotation after pH value to neutrality is adjusted after stirring
Turn in evaporimeter, 60~80min is concentrated under conditions of revolving speed is 250~300r/min and temperature is 50~70 DEG C, modification is made
Dispersing agent；According to parts by weight, by 20~22 parts of above-mentioned modifiers dispersants, 2~3 parts of aluminium oxide, 4~6 parts of silica, 4~5 parts
Magnesia is put into blender, is stirred 50 in the revolving speed that temperature is 45~55 DEG C and speed of agitator is 500~600r/min
Filter residue is obtained by filtration in~60min after stirring, filter residue 3~5 times is wash with distilled water up to hybrid solid product；By above-mentioned mixing
Solid product and distilled water are in 1:10 investment reaction kettle in mass ratio, and it is 10~12% that mass fraction is added dropwise into reaction kettle
Sodium hydroxide solution adjusts pH value to 11~12, and 30~40min is mixed with the revolving speed of 300~400r/min with blender,
Reactor temperature is increased to 120~130 DEG C of 40~50min of isothermal reaction after stirring, filter residue is obtained by filtration after reaction, with steaming
Distilled water is cleaned filter residue 3~5 times, is put into baking oven, dry 3~4h discharging ground 50 under conditions of temperature is 110~120 DEG C
Mesh is up to epigranular high stable houghite.
Embodiment 1
The preparation of mixed serum:
It is in mass ratio in 5:1 investment vacuum oven, in the item that temperature is 50 DEG C and vacuum degree is 100Pa by bean dregs and starch
Dry 3h obtains dried material under part, is in mass ratio that 1:10 is put into high-temperature high-pressure reaction kettle by dried material and distilled water,
Air pressure in reaction kettle is increased to 0.5MPa, temperature is increased to 115 DEG C, and constant temperature and pressure reacts 40min and reaction mixture is made；
It is in mass ratio to place the beaker water in 5:1 investment beaker by the hydrochloric acid that above-mentioned reaction mixture and mass fraction are 10%
In the water-bath that bath temperature is 40 DEG C, 40min is mixed with the revolving speed of 300r/min with blender, acid mixed solution is made, to
The aluminum chloride powder of acid mixed solution quality 6% is added in beaker, continues to stir the obtained mixed serum of 30min；
The preparation of modifiers dispersants:
6% potassium permanganate powder of mixed serum quality is added into above-mentioned beaker, places the beaker in sonic oscillation instrument, in frequency
Oxidation liquid is made for oscillation mixing 30min under conditions of 36kHz, the sulfuric acid for being 15% by oxidation liquid and mass fraction
Solution is to be uniformly mixed to be made to reaction solution in 5:1 investment three-necked flask in mass ratio；
The ethylene glycol solution for being 30% to the mass fraction of reaction solution quality 20% is added into above-mentioned three-necked flask, by three-necked flask
It is placed in resistance heating set, temperature in heating mantle is increased to 60 DEG C, with blender with the revolving speed of 500r/min under constant temperature
2h is stirred, is put into Rotary Evaporators after pH value to neutrality is adjusted after stirring, in revolving speed be 250r/min and temperature is 50 DEG C
Under the conditions of concentration 60min be made modifiers dispersants；
The preparation of epigranular high stable houghite:
According to parts by weight, 20 parts of above-mentioned modifiers dispersants, 2 parts of aluminium oxide, 4 parts of silica, 4 parts of magnesia are put into blender
In, it is stirred 50min in the revolving speed that temperature is 45 DEG C and speed of agitator is 500r/min, filter residue is obtained by filtration after stirring, uses
Distilled water cleans filter residue 3 times up to hybrid solid product；
It is in mass ratio that quality point is added dropwise into reaction kettle in 1:10 investment reaction kettle by above-mentioned hybrid solid product and distilled water
Number adjusts pH value to 11 for 10% sodium hydroxide solution, and 30min, stirring is mixed with the revolving speed of 300r/min with blender
Reactor temperature is increased to 120 DEG C of isothermal reaction 40min afterwards, filter residue is obtained by filtration after reaction, wash with distilled water filter residue 3
It is secondary, it puts into baking oven, dry 3h discharges ground 50 mesh up to epigranular high stable class under conditions of temperature is 110 DEG C
Hydrotalcite.
Embodiment 2
The preparation of mixed serum:
It is in mass ratio in 5:1 investment vacuum oven, in the item that temperature is 55 DEG C and vacuum degree is 150Pa by bean dregs and starch
Dry 3.5h obtains dried material under part, is in mass ratio 1:10 investment high-temperature high-pressure reaction kettle by dried material and distilled water
In, air pressure in reaction kettle is increased to 0.6MPa, temperature is increased to 120 DEG C, and constant temperature and pressure reacts 45min and reaction mixing is made
Liquid；
It is in mass ratio to place the beaker water in 5:1 investment beaker by the hydrochloric acid that above-mentioned reaction mixture and mass fraction are 12%
In the water-bath that bath temperature is 45 DEG C, 45min is mixed with the revolving speed of 350r/min with blender, acid mixed solution is made, to
The aluminum chloride powder of acid mixed solution quality 7% is added in beaker, continues to stir the obtained mixed serum of 35min；
The preparation of modifiers dispersants:
8% potassium permanganate powder of mixed serum quality is added into above-mentioned beaker, places the beaker in sonic oscillation instrument, in frequency
Oxidation liquid is made for oscillation mixing 35min under conditions of 38kHz, the sulfuric acid for being 17% by oxidation liquid and mass fraction
Solution is to be uniformly mixed to be made to reaction solution in 5:1 investment three-necked flask in mass ratio；
The ethylene glycol solution for being 32% to the mass fraction of reaction solution quality 25% is added into above-mentioned three-necked flask, by three-necked flask
It is placed in resistance heating set, temperature in heating mantle is increased to 65 DEG C, with blender with the revolving speed of 520r/min under constant temperature
2.5h is stirred, is put into Rotary Evaporators after pH value to neutrality is adjusted after stirring, in revolving speed be 270r/min and temperature is 60 DEG C
Under conditions of concentration 70min be made modifiers dispersants；
The preparation of epigranular high stable houghite:
According to parts by weight, 21 parts of above-mentioned modifiers dispersants, 2 parts of aluminium oxide, 5 parts of silica, 4 parts of magnesia are put into blender
In, it is stirred 55min in the revolving speed that temperature is 50 DEG C and speed of agitator is 550r/min, filter residue is obtained by filtration after stirring, uses
Distilled water cleans filter residue 4 times up to hybrid solid product；
It is in mass ratio that quality point is added dropwise into reaction kettle in 1:10 investment reaction kettle by above-mentioned hybrid solid product and distilled water
Number adjusts pH value to 11 for 11% sodium hydroxide solution, and 35min, stirring is mixed with the revolving speed of 350r/min with blender
Reactor temperature is increased to 125 DEG C of isothermal reaction 45min afterwards, filter residue is obtained by filtration after reaction, wash with distilled water filter residue 4
It is secondary, it puts into baking oven, dry 3.5h discharges ground 50 mesh up to epigranular high stable under conditions of temperature is 115 DEG C
Houghite.
Embodiment 3
The preparation of mixed serum:
It is in mass ratio in 5:1 investment vacuum oven, in the item that temperature is 60 DEG C and vacuum degree is 200Pa by bean dregs and starch
Dry 4h obtains dried material under part, is in mass ratio that 1:10 is put into high-temperature high-pressure reaction kettle by dried material and distilled water,
Air pressure in reaction kettle is increased to 0.7MPa, temperature is increased to 125 DEG C, and constant temperature and pressure reacts 50min and reaction mixture is made；
It is in mass ratio to place the beaker water in 5:1 investment beaker by the hydrochloric acid that above-mentioned reaction mixture and mass fraction are 15%
In the water-bath that bath temperature is 50 DEG C, 50min is mixed with the revolving speed of 400r/min with blender, acid mixed solution is made, to
The aluminum chloride powder of acid mixed solution quality 8% is added in beaker, continues to stir the obtained mixed serum of 40min；
The preparation of modifiers dispersants:
10% potassium permanganate powder of mixed serum quality is added into above-mentioned beaker, places the beaker in sonic oscillation instrument, in frequency
Oxidation liquid is made for oscillation mixing 40min under conditions of 40kHz, the sulfuric acid for being 20% by oxidation liquid and mass fraction
Solution is to be uniformly mixed to be made to reaction solution in 5:1 investment three-necked flask in mass ratio；
The ethylene glycol solution for being 35% to the mass fraction of reaction solution quality 30% is added into above-mentioned three-necked flask, by three-necked flask
It is placed in resistance heating set, temperature in heating mantle is increased to 70 DEG C, with blender with the revolving speed of 550r/min under constant temperature
3h is stirred, is put into Rotary Evaporators after pH value to neutrality is adjusted after stirring, in revolving speed be 300r/min and temperature is 70 DEG C
Under the conditions of concentration 80min be made modifiers dispersants；
The preparation of epigranular high stable houghite:
According to parts by weight, 22 parts of above-mentioned modifiers dispersants, 3 parts of aluminium oxide, 6 parts of silica, 5 parts of magnesia are put into blender
In, it is stirred 60min in the revolving speed that temperature is 55 DEG C and speed of agitator is 600r/min, filter residue is obtained by filtration after stirring, uses
Distilled water cleans filter residue 5 times up to hybrid solid product；
It is in mass ratio that quality point is added dropwise into reaction kettle in 1:10 investment reaction kettle by above-mentioned hybrid solid product and distilled water
Number adjusts pH value to 12 for 12% sodium hydroxide solution, and 40min, stirring is mixed with the revolving speed of 400r/min with blender
Reactor temperature is increased to 130 DEG C of isothermal reaction 50min afterwards, filter residue is obtained by filtration after reaction, wash with distilled water filter residue 5
It is secondary, it puts into baking oven, dry 4h discharges ground 50 mesh up to epigranular high stable class under conditions of temperature is 120 DEG C
Hydrotalcite.
Comparative example 1: it is essentially identical with the preparation method of embodiment 2, it has only the difference is that lacking mixed serum.
Comparative example 2: it is essentially identical with the preparation method of embodiment 2, it has only the difference is that lacking modifiers dispersants.
Comparative example 3: the epigranular high stable houghite of Shandong company production.
Partial size test characterizes the pattern of sample using JSM-6700F field emission scanning electron microscope (SEM), measures partial size
Size.
Table 1: houghite performance measurement result
| Detection project | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Partial size (nm) | 25 | 22 | 20 | 150 | 170 | 140 |
| Repeatability | It is good | It is good | It is good | Difference | Difference | Difference |
In summary, houghite uniform particle diameter of the invention as can be seen from Table 1, good dispersion, batch is reproducible, durable
Property it is good, have broad prospect of application.
The foregoing is merely preferred modes of the invention, are not intended to limit the invention, all in spirit and original of the invention
Within then, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of preparation method of epigranular high stable houghite, it is characterised in that specific preparation step are as follows:
(1) by modifiers dispersants, aluminium oxide, silica, magnesia investment blender, in temperature be 45~55 DEG C and stirring turns
Speed is that the revolving speed of 500~600r/min is stirred 50~60min, filter residue is obtained by filtration after stirring, wash with distilled water filter residue 3
~5 times up to hybrid solid product；
(2) by hybrid solid product and distilled water investment reaction kettle, the hydrogen that mass fraction is 10~12% is added dropwise into reaction kettle
Sodium hydroxide solution adjusts pH value to 11~12, and 30~40min is mixed with the revolving speed of 300~400r/min with blender, stirs
Reactor temperature is increased to 120~130 DEG C of 40~50min of isothermal reaction after mixing, filter residue is obtained by filtration after reaction, with distillation
Water cleans filter residue 3~5 times, puts into baking oven, ground 50 mesh of dry 3~4h discharging under conditions of temperature is 110~120 DEG C
It sieves up to epigranular high stable houghite；
The specific preparation step of the mixed serum are as follows:
(1) bean dregs and starch are put into vacuum oven, in the item that temperature is 50~60 DEG C and vacuum degree is 100~200Pa
Dry 3~4h obtains dried material under part, is in mass ratio 1:10 investment high-temperature high-pressure reaction kettle by dried material and distilled water
In, air pressure in reaction kettle is increased to 0.5~0.7MPa, temperature is increased to 115~125 DEG C, and constant temperature and pressure reacts 40~50min
Reaction mixture is made；
(2) hydrochloric acid that reaction mixture and mass fraction are 10~15% is put into beaker, placing the beaker bath temperature is 40
In~50 DEG C of water-bath, 40~50min is mixed with the revolving speed of 300~400r/min with blender, acidic mixed is made
Aluminum chloride powder is added into beaker for liquid, continues 30~40min of stirring and mixed serum is made；
The specific preparation step of the modifiers dispersants are as follows:
(1) potassium permanganate powder is added into beaker, places the beaker in sonic oscillation instrument, in the item that frequency is 36~40kHz
Oxidation liquid is made in 30~40min of oscillation mixing under part, the sulfuric acid solution for being 15~20% by oxidation liquid and mass fraction
It puts into be uniformly mixed in three-necked flask and be made to reaction solution；
(2) ethylene glycol solution for being 30~35% to the mass fraction of reaction solution quality 20~30% is added into three-necked flask, it will
Three-necked flask is placed in resistance heating set, and temperature in heating mantle is increased to 60~70 DEG C, with blender with 500 under constant temperature
The revolving speed of~550r/min stirs 2~3h, puts into Rotary Evaporators after pH value to neutrality is adjusted after stirring, is 250 in revolving speed
Modifiers dispersants are made in 60~80min of concentration under conditions of~300r/min and temperature are 50~70 DEG C.
2. a kind of preparation method of epigranular high stable houghite according to claim 1, it is characterised in that: preferably
According to parts by weight, the modifiers dispersants are 20~22 parts, aluminium oxide is 2~3 parts, silica is 4~6 parts, oxidation
Magnesium is 4~5 parts.
3. a kind of preparation method of epigranular high stable houghite according to claim 1, it is characterised in that: described
Hybrid solid product and distilled water mass ratio be 1:10.
4. a kind of preparation method of epigranular high stable houghite according to claim 1, it is characterised in that: mixing
The mass ratio of bean dregs described in the specific preparation step (1) of slurries and starch is 5:1.
5. a kind of preparation method of epigranular high stable houghite according to claim 1, it is characterised in that: mixing
The mass ratio for the hydrochloric acid that reaction mixture described in the specific preparation step (1) of slurries and mass fraction are 10~15% is 5:
1。
6. a kind of preparation method of epigranular high stable houghite according to claim 1, it is characterised in that: mixing
The quality for the aluminum chloride powder being added described in the specific preparation step (1) of slurries into beaker is acid mixed solution quality
6~8%.
7. a kind of preparation method of epigranular high stable houghite according to claim 1, it is characterised in that: modified
The quality for the potassium permanganate powder being added described in the specific preparation step (1) of dispersing agent into beaker is mixed serum quality
6~10%.
8. a kind of preparation method of epigranular high stable houghite according to claim 1, it is characterised in that: modified
The quality for the sulfuric acid solution that oxidation liquid described in the specific preparation step (1) of dispersing agent and mass fraction are 15~20%
Than for 5:1.
9. a kind of preparation method of epigranular high stable houghite according to claim 1, it is characterised in that: modified
The ethylene glycol that the mass fraction being added described in the specific preparation step (1) of dispersing agent into three-necked flask is 30~35% is molten
The quality of liquid is 20~30% to reaction solution quality.
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| CN113121043A (en) * | 2019-12-30 | 2021-07-16 | 湖北金汉江精制棉有限公司 | Purified cotton wastewater recycling system |
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| CN115246971B (en) * | 2021-12-30 | 2023-05-16 | 邵阳学院 | Preparation method of modified hydrocalumite-bean dregs for PVC heat stabilizer |
| CN115536907A (en) * | 2022-09-15 | 2022-12-30 | 呈和科技股份有限公司 | Special hydrotalcite additive for agricultural film and application thereof |
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