CN110339680A - A kind of preparation method of high absorption impervious drying agent for containers material - Google Patents
A kind of preparation method of high absorption impervious drying agent for containers material Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of high absorption impervious drying agent for containers material, belong to desiccant technical field.Technical solution of the present invention uses sol-gel method and is prepared for cordierite powder, the colloidal crystal template with ordered 3 D structure is assembled into using mono-dispersion microballoon, pass through the filling of precursor, cleaning, the processes such as sintering, uniform particle diameter is prepared, and the cordierite material with three-dimensional order dispersed nano aperture, the zeolite membrane material that technical solution of the present invention is coated in material internal, the optimum porosity that material after cladding has is by coating modification, improve the hole intensity of material, since zeolite membrane material surface texture is spongy meso-hole structure, there is meso-hole structure with running through, and the spherical particle with the structure is throughout entire sample, since duct is smaller, attqched tension is bigger, it further increases material and is retained impervious performance.
Description
Technical field
The present invention relates to a kind of preparation methods of high absorption impervious drying agent for containers material, belong to desiccant technology neck
Domain.
Background technique
With economic sustainable development, effect of the Container Transport in cargo transport will protrusion more.But collect
Vanning can generate the phenomenon that a kind of " container rain " during transportation, and this phenomenon frequently occurs in container transport by sea
Cheng Zhong.The presence of " container rain " can not only corrode the metal cabinet for constituting container, also can to freight in container
Cause burn into dampness, mildew etc..The common method for solving " container rain " is the water absorbed in container using desiccant
Point, keep the low-humidity environment of internal container.Container often mainly has calcium chloride, silica gel and molecular sieve etc. with desiccant.So
And these common desiccant are haveed the defects that different in use, with the development of economy, are increasingly difficult to adapt to modern
Change the demand of drying agent for containers.Anhydrous calcium chloride granule strength is small, and particle is easy to crush after water suction, dity cargo；And it stores up
Water divides ability low, sepage phenomenon easily occurs；Silica-gel desiccant water absorption rate is smaller, and maximum water absorption rate is 30% or so, and price
Valuableness is not suitable for a wide range of use；A large amount of heat is released after quick lime water suction, reacting to generate with water has the strong of strong corrosive
Alkali.
Due to the characteristic of container sealing and the difference of various regions weather, internal container day and night temperature may be up to 20 DEG C of left sides
It is right.Container daytime is caused temperature to increase by the irradiation of tropical sun, moisture is evaporated, and then diffused in each of internal container
Corner；Nocturnal temperature decline, moisture is liquefied as droplet, is attached to cargo and container surface, to cause the damage of damp of cargo.?
The generation condensation and vaporization of moisture again and again, occur serious corrosion to cargo and container surface and invade in transportational process
Evil.
In the use, transport and storing process of article, guarantees the drying of article commonly using various desiccant, avoid
It is moist, mouldy, corrosion phenomena such as generation.Desiccant is also known as water absorbing agent, adsorbent etc., is inhaled by its stronger water absorbing properties
Moisture in attached specific environment keeps the drying of particular space long period, achievees the purpose that moisture-proof, mould proof.
All kinds of desiccant are different because of its application field of unique performance and design feature in real life.Example
Such as, the inside of silica-gel desiccant is superfine pore reticular structure, can be widely applied to container, electronic product, leather, medicine
The industries such as food；Mineral agent is usually the safe and nontoxic harmless and degradable ring being prepared based on natural materials
Guarantor's type desiccant, mineral agent absorption property under room temperature and general humidity is good, be widely used in security requirement compared with
In the high and product for oil sealing, gas phase cannot to be used to seal up for safekeeping, such as precision optical instrument and advanced electronic product, medical health care medicine
Drying in product and food pack；For anhydrous calcium chloride because inexpensive, drying capacity is strong, rate of drying is fast, can regenerate, but the moisture absorption is easy
Become solution, generally to fill drier and drying tower, dry drug and multiple gases.
According to the difference of drying mode, drying is divided into static dry and dynamic drying.Warehouse, pharmaceutical factory, precision machinery, electricity
Sub- equipment manufactory, instrument air drying etc., mostly use static drying mode；Hydrogen, oxygen, nitrogen, CO2, acetylene, ethylene,
Methane, SO3、SO2, natural gas etc., such material mostly uses dynamic drying mode.Static drying be the quantitative desiccant of selection and
Moist medium comes into full contact with and moisture achievees the purpose that removal moisture drying in adsorbing medium.Dynamic drying is a certain amount of drying of selection
Agent is filled in adsorption column, the certain fluid to be dried of concentration is flowed through adsorption column under certain condition, moisture is adsorbed column
Middle desiccant adsorbs and achievees the purpose that removal moisture drying.
It is different according to desiccant suction type, desiccant can be divided into physical absorption desiccant and chemisorption desiccant.
The adsorption process as caused by the active force between adsorbate and the molecular link of adsorbent is referred to as physical absorption or Van der Waals absorption,
The active force of absorption is caused to be known as Van der Waals force.Chemisorption is formation sorption chemical key between adsorbent and adsorption molecule
Process in adsorption process, has occurred the transfer between electronics, exchanges and shared between adsorbent and adsorbate.Adsorbent surface
Force distribution it is uneven, surface atom it is extra at bonding force by absorption air in gas molecule reaches balance.Chemistry is inhaled
Attached that mono layer adsorption only occurs, heat of adsorption is suitable with chemical reaction heat, and is mostly Irreversible Adsorption.
Conventional dry drying prescription is mostly that single raw material is made, and according to the moisture pick-up properties that various features are shown, be can satisfy
The moisture-proof purpose of the moisture absorption in some fields, but there is also some defects.Such as: due to acid-base neutralization reaction, acid and alkalinity is dry
Agent cannot dry incompatible gas and liquid therewith；Silica-gel desiccant water absorption rate is lower；Anhydrous calcium chloride desiccant moisture absorption
Rate is higher, but be easy to happen sepage etc..It is higher for requiring hydroscopicity, and the dehumidifying of the article of moisture absorption environment harshness, study people
Member had studied various new composite drying agent in recent years, achieved the purpose that dehumidify in complex condition.
Compared with the desiccant that uses of tradition, the characteristics of novel drier is: (1) novel drier is no longer single substance
It constitutes, but is formed by many kinds of substance by different process combinations；(2) forming the substance of novel drier is mainly natural mine
Substance or natural high molecular substance；(3) after the water suction of part novel drier, it can obtain out whether desiccant absorbs water by external table
Reach saturation；(4) novel drier has preferable water storage effect.The characteristics of these desiccant are mainly for " container rain " and
Design has specificity, but is mostly external manufacturer's production, and the country is at present to the research of container special drying agent also in spy
Rope and conceptual phase, and the development trend of desiccant will develop towards the direction of more specialized, high-hydroscopicity and environment-friendly type.
Summary of the invention
The technical problems to be solved by the invention: it aiming at the problem that existing drying agent for containers easily sepage occurs, provides
A kind of preparation method of high absorption impervious drying agent for containers material.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
(1) according to parts by weight, 45~50 parts of deionized waters, 10~15 parts of styrene, 3~5 parts of sodium bicarbonates, 6 are weighed respectively
~8 parts of methyl methacrylates and 1~2 part of 1% ammonium persulfate solution of mass fraction are placed in three-necked flask, are stirred and are protected
Temperature reaction, ultrasonic disperse obtain dispersion microsphere lotion；It collects dispersion microsphere lotion and stands isothermal holding in an oven, collect
Dry crystal template；
(2) in mass ratio 1: 10, dry crystal template is added in hydrophobic silicone oil, ramped heating schedule processing, Heat preservation,
Filter and collect filter cake, washing, dry matrix template particles；According to parts by weight, respectively weigh 45~50 parts of dehydrated alcohols,
10~15 parts of 5% magnesium nitrate solutions of mass fraction, 10~15 parts of 5% aluminum nitrate solutions of mass fraction, 3~5 parts of ethyl orthosilicates,
1~2 part of 10% nitric acid of mass fraction and 65~80 parts of deionized waters are placed in conical flask, are stirred and are stood to obtain presoma
Matrix template particles are dipped in precursor solution by solution, stand, filter and collect filter cake, washing, dry, collection drying
Particle and isothermal holding, heating heating, keep the temperature calcination processing, and standing is cooled to room temperature, and grinding distribution sieving obtains binding matrix
Grain；
(3) according to parts by weight, respectively weigh 45~50 parts of deionized waters, 10~15 parts of tetrapropylammonium hydroxide, 1~2 part receive
Rice silica, 0.1~0.2 part of nano-titanium dioxide are placed in three-necked flask, are stirred simultaneously decentralized processing, are obtained reaction solution simultaneously
In mass ratio 1: 25,15% hydrogenperoxide steam generator of mass fraction is added dropwise in reaction solution, after being added dropwise to complete, is stirred simultaneously
It being placed in reaction kettle, Crystallizing treatment, is centrifugated and collects lower sediment, washing, dry, heat preservation calcining remove impurity treatment,
After standing is cooled to room temperature, matrix desiccant is obtained；
(4) according to parts by weight, 45~50 parts of matrix desiccant, 3~5 parts of calcium chloride, 6~8 parts of microcrystalline celluloses are weighed respectively
It is placed in mortar, grinding distribution sieving obtains sieving particle, then in mass ratio 1: 25, by 20% bromthymol blue second of mass fraction
Alcoholic solution is added in sieving particle, is stirred and is dried, grinds granulation balling-up, and the high absorption can be prepared into
Impervious drying agent for containers material.
In the isothermal holding of standing in an oven oven conditions be humidity be 50%, temperature is 50 DEG C.
The ramped heating schedule processing is, by 3 DEG C/min, heating is heated to heating at 55~60 DEG C, and heat preservation adds
2~3h of heat.
Described is dry that matrix template particles are successively to clean 3~5 with n-hexane, dehydrated alcohol and isopropanol respectively
Secondary, vacuum freeze drying obtains matrix template particles.
The described heating heating, heat preservation calcination processing are heated to 850~900 DEG C by 5 DEG C/min heating, and heat preservation calcines 3~
5h。
The hydrogenperoxide steam generator drop rate is 2~3mL/min.
The binding matrix grain diameter is 500 mesh.
The Crystallizing treatment be in 150~160 DEG C of reaction kettles and steam crystallization 20~for 24 hours.
The heat preservation calcining removal impurity treatment temperature is 850~900 DEG C.
The present invention is compared with other methods, and advantageous effects are:
Technical solution of the present invention uses sol-gel method and is prepared for cordierite powder, and being assembled into using mono-dispersion microballoon is had
The colloidal crystal template of ordered 3 D structure has prepared uniform particle diameter by processes such as the fillings, cleaning, sintering of precursor,
And the cordierite material with three-dimensional order dispersed nano aperture, this 3-D ordered multiporous cordierite nano material are opposite
Existing nanoscale cordierite powder has better monodispersity and more stable shape and structure, compared to existing honeycomb
Shape cordierite catalyst carrier has bigger specific surface area, it is brilliant known to basis material cordierite powder material structure
The interior presence due to a large amount of ducts, so that cordierite powder material has biggish specific surface, surface-active also with higher
And it is able to carry out the ability of physical absorption and chemisorption simultaneously, therefore be the good raw material for substituting conventional dry drying prescription, with biography
System desiccant is compared, and cordierite powder material producing process is simple, quality-high and inexpensive, and cordierite powder material is environmentally friendly original
Material, nontoxic and pollution-free, cordierite powder material itself is stronger to the adsorption capacity of water, and water imbibition is preferable, by making its absorption
Active site increases, and effectively coats simultaneously load molecular sieve material by enhancing water absorbency and water retentivity, while on its surface, passes through
Activity more superior than powder catalyst is shown in terms of adsorbing with moisture-absorption water-retention with 3-D ordered multiporous molecular screen material,
This is because nanoscale hole configurations is in the specific surface area realization hydrone and zeolite membrane material for being capable of increasing catalyst
While coming into full contact with, realize that hydrone is filled inside molecular sieve and comparatively closely combined in hole range, into one
Step improves the water retention property of material, due to the zeolite membrane material that technical solution of the present invention is coated in material internal, molecular screen membrane
Close-packed arrays, intracrystalline pore are reduced between layer crystal body, are contacted when hydrone passes through molecular sieve pore passage with more active sites, thus
It is that hydrone and material surface binding performance enhance, while the effective of zeolite membrane material coats and crystallize filling to material internal
Technical solution, the optimum porosity that cladding has on material pore interior, due to the material after cladding by coating modification,
The hole intensity for improving material, since zeolite membrane material surface texture is spongy meso-hole structure, having to run through has mesoporous knot
Structure, and there is the spherical particle of the structure throughout entire sample, since duct is smaller, attqched tension is bigger, further increases material
Material is retained impervious performance.
Specific embodiment
According to parts by weight, 45~50 parts of deionized waters, 10~15 parts of styrene, 3~5 parts of sodium bicarbonates, 6 are weighed respectively
~8 parts of methyl methacrylates and 1~2 part of 1% ammonium persulfate solution of mass fraction are placed in three-necked flask, are stirred juxtaposition
2~3h of insulation reaction at 85~95 DEG C, 10~15min of ultrasonic disperse obtain dispersion microsphere lotion；Collect dispersion microsphere lotion simultaneously
It is placed in that humidity is 50%, temperature is in 50 DEG C of baking ovens, after standing isothermal holding 20~for 24 hours, collects to obtain dry crystal template；By matter
Ratio 1: 10 is measured, dry crystal template is added in hydrophobic silicone oil, is stirred and by 3 DEG C/min, heats up and is heated to 55~60
Heat at DEG C, after 2~3h of Heat preservation, filters and collect filter cake, successively use n-hexane, dehydrated alcohol and isopropanol respectively
Cleaning 3~5 times, vacuum freeze drying obtains matrix template particles；According to parts by weight, respectively weigh 45~50 parts of dehydrated alcohols,
10~15 parts of 5% magnesium nitrate solutions of mass fraction, 10~15 parts of 5% aluminum nitrate solutions of mass fraction, 3~5 parts of ethyl orthosilicates,
1~2 part of 10% nitric acid of mass fraction and 65~80 parts of deionized waters are placed in conical flask, are stirred and are stood to obtain presoma
Matrix template particles are dipped in precursor solution by solution, in mass ratio 1: 10, after standing 40~48h, are filtered and are collected filter
Cake, after being rinsed 3~5 times with dehydrated alcohol, vacuum drying 20~for 24 hours, collection dry particle, which is placed at 100~110 DEG C, to be kept the temperature
25~30min is handled, then is heated to 850~900 DEG C by 5 DEG C/min heating, after 3~5h is calcined in heat preservation, standing is cooled to room temperature,
Grinding distribution crosses 500 meshes, obtains binding matrix particle；According to parts by weight, 45~50 parts of deionized waters, 10~15 are weighed respectively
Part tetrapropylammonium hydroxide, 1~2 part of nano silica, 0.1~0.2 part of nano-titanium dioxide are placed in three-necked flask, are stirred
Simultaneously 10~15min of decentralized processing is mixed, reaction solution and in mass ratio 1: 25 are obtained, 15% hydrogenperoxide steam generator of mass fraction is added dropwise
Into reaction solution, control drop rate is that 2~3mL/min is stirred and is placed in reaction kettle after being added dropwise to complete, 150
In~160 DEG C of reaction kettles and steam crystallization 20~for 24 hours, it is centrifugated and is collected lower sediment, is rinsed with deionized water to washing
It is quiet after 25~30min of heat preservation calcining after liquid is in neutrality, then at 100~110 DEG C after drying to constant weight, then at 850~900 DEG C
It sets after being cooled to room temperature, obtains matrix desiccant；According to parts by weight, 45~50 parts of matrix desiccant, 3~5 parts of chlorine are weighed respectively
Change calcium, 6~8 parts of microcrystalline celluloses are placed in mortar, and grinding distribution crosses 200 meshes, obtain sieving particle, then in mass ratio 1: 25,
20% bromthymol blue ethanol solution of mass fraction is added in sieving particle, is stirred and dries, grind granulation
Balling-up can be prepared into the high absorption impervious drying agent for containers material.
Example 1
According to parts by weight, 45 parts of deionized waters, 10 parts of styrene, 3 parts of sodium bicarbonates, 6 parts of methyl methacrylates are weighed respectively
Ester and 1 part of 1% ammonium persulfate solution of mass fraction are placed in three-necked flask, are stirred and are placed in insulation reaction 2h at 85 DEG C,
Ultrasonic disperse 10min obtains dispersion microsphere lotion；It collects dispersion microsphere lotion and is placed in that humidity is 50%, temperature is 50 DEG C of baking ovens
In, after standing isothermal holding 20h, collect to obtain dry crystal template；In mass ratio 1: 10, dry crystal template is added to hydrophobic
It in silicone oil, is stirred and by 3 DEG C/min, heating is heated to heating at 55 DEG C, after Heat preservation 2h, filters and collects filter
Cake, difference are successively cleaned 3 times with n-hexane, dehydrated alcohol and isopropanol, and vacuum freeze drying obtains matrix template particles；By weight
It is molten to weigh 45 parts of dehydrated alcohols, 10 parts of 5% magnesium nitrate solutions of mass fraction, 10 parts of 5% aluminum nitrates of mass fraction respectively for number meter
Liquid, 3 parts of ethyl orthosilicates, 1 part of 10% nitric acid of mass fraction and 65 parts of deionized waters are placed in conical flask, are stirred and quiet
Precursor solution, in mass ratio 1: 10 are set to obtain, matrix template particles are dipped in precursor solution, after standing 40h, filtering is simultaneously
Filter cake is collected, after being rinsed 3 times with dehydrated alcohol, is dried in vacuo 20h, dry particle is collected and is placed in isothermal holding at 100 DEG C
25min, then 850 DEG C are heated to by 5 DEG C/min heating, after 3h is calcined in heat preservation, standing is cooled to room temperature, and grinding distribution crosses 500 mesh
Sieve, obtains binding matrix particle；According to parts by weight, respectively weigh 45 parts of deionized waters, 10 parts of tetrapropylammonium hydroxide, 1 part receive
Rice silica, 0.1 part of nano-titanium dioxide are placed in three-necked flask, are stirred simultaneously decentralized processing 10min, are obtained reaction solution simultaneously
In mass ratio 1: 25,15% hydrogenperoxide steam generator of mass fraction is added dropwise in reaction solution, control drop rate is 2mL/min,
It after being added dropwise to complete, is stirred and is placed in reaction kettle, with steam crystallization 20h in 150 DEG C of reaction kettles, be centrifugated and receive
Collect lower sediment, rinsed with deionized water to cleaning solution after being in neutrality, then dries at 100 DEG C to constant weight, then at 850 DEG C,
After heat preservation calcining 25min, after standing is cooled to room temperature, matrix desiccant is obtained；According to parts by weight, it is dry that 45 parts of matrixes are weighed respectively
Drying prescription, 3 parts of calcium chloride, 6 parts of microcrystalline celluloses are placed in mortar, and grinding distribution crosses 200 meshes, obtain sieving particle, then press quality
Than 1: 25,20% bromthymol blue ethanol solution of mass fraction is added in sieving particle, is stirred and dries, grounds travel
Broken granulation balling-up can be prepared into the high absorption impervious drying agent for containers material.
Example 2
According to parts by weight, 47 parts of deionized waters, 12 parts of styrene, 4 parts of sodium bicarbonates, 7 parts of methyl methacrylates are weighed respectively
Ester and 1 part of 1% ammonium persulfate solution of mass fraction are placed in three-necked flask, are stirred and are placed in insulation reaction 2h at 90 DEG C,
Ultrasonic disperse 12min obtains dispersion microsphere lotion；It collects dispersion microsphere lotion and is placed in that humidity is 50%, temperature is 50 DEG C of baking ovens
In, after standing isothermal holding 22h, collect to obtain dry crystal template；In mass ratio 1: 10, dry crystal template is added to hydrophobic
It in silicone oil, is stirred and by 3 DEG C/min, heating is heated to heating at 58 DEG C, after Heat preservation 2h, filters and collects filter
Cake, difference are successively cleaned 4 times with n-hexane, dehydrated alcohol and isopropanol, and vacuum freeze drying obtains matrix template particles；By weight
It is molten to weigh 47 parts of dehydrated alcohols, 12 parts of 5% magnesium nitrate solutions of mass fraction, 12 parts of 5% aluminum nitrates of mass fraction respectively for number meter
Liquid, 4 parts of ethyl orthosilicates, 1 part of 10% nitric acid of mass fraction and 75 parts of deionized waters are placed in conical flask, are stirred and quiet
Precursor solution, in mass ratio 1: 10 are set to obtain, matrix template particles are dipped in precursor solution, after standing 44h, filtering is simultaneously
Filter cake is collected, after being rinsed 4 times with dehydrated alcohol, is dried in vacuo 22h, dry particle is collected and is placed in isothermal holding at 105 DEG C
28min, then 875 DEG C are heated to by 5 DEG C/min heating, after 4h is calcined in heat preservation, standing is cooled to room temperature, and grinding distribution crosses 500 mesh
Sieve, obtains binding matrix particle；According to parts by weight, respectively weigh 47 parts of deionized waters, 12 parts of tetrapropylammonium hydroxide, 1 part receive
Rice silica, 0.1 part of nano-titanium dioxide are placed in three-necked flask, are stirred simultaneously decentralized processing 12min, are obtained reaction solution simultaneously
In mass ratio 1: 25,15% hydrogenperoxide steam generator of mass fraction is added dropwise in reaction solution, control drop rate is 2mL/min,
It after being added dropwise to complete, is stirred and is placed in reaction kettle, with steam crystallization 22h in 155 DEG C of reaction kettles, be centrifugated and receive
Collect lower sediment, rinsed with deionized water to cleaning solution after being in neutrality, then dries at 105 DEG C to constant weight, then at 875 DEG C,
After heat preservation calcining 28min, after standing is cooled to room temperature, matrix desiccant is obtained；According to parts by weight, it is dry that 47 parts of matrixes are weighed respectively
Drying prescription, 4 parts of calcium chloride, 7 parts of microcrystalline celluloses are placed in mortar, and grinding distribution crosses 200 meshes, obtain sieving particle, then press quality
Than 1: 25,20% bromthymol blue ethanol solution of mass fraction is added in sieving particle, is stirred and dries, grounds travel
Broken granulation balling-up can be prepared into the high absorption impervious drying agent for containers material.
Example 3
According to parts by weight, 50 parts of deionized waters, 15 parts of styrene, 5 parts of sodium bicarbonates, 8 parts of methyl methacrylates are weighed respectively
Ester and 2 parts of 1% ammonium persulfate solutions of mass fraction are placed in three-necked flask, are stirred and are placed in insulation reaction 3h at 95 DEG C,
Ultrasonic disperse 15min obtains dispersion microsphere lotion；It collects dispersion microsphere lotion and is placed in that humidity is 50%, temperature is 50 DEG C of baking ovens
In, after standing isothermal holding for 24 hours, collect to obtain dry crystal template；In mass ratio 1: 10, dry crystal template is added to hydrophobic
It in silicone oil, is stirred and by 3 DEG C/min, heating is heated to heating at 60 DEG C, after Heat preservation 3h, filters and collects filter
Cake, difference are successively cleaned 5 times with n-hexane, dehydrated alcohol and isopropanol, and vacuum freeze drying obtains matrix template particles；By weight
It is molten to weigh 50 parts of dehydrated alcohols, 15 parts of 5% magnesium nitrate solutions of mass fraction, 15 parts of 5% aluminum nitrates of mass fraction respectively for number meter
Liquid, 5 parts of ethyl orthosilicates, 2 parts of 10% nitric acid of mass fraction and 80 parts of deionized waters are placed in conical flask, are stirred and quiet
Precursor solution, in mass ratio 1: 10 are set to obtain, matrix template particles are dipped in precursor solution, after standing 48h, filtering is simultaneously
Filter cake is collected, after being rinsed 5 times with dehydrated alcohol, vacuum drying for 24 hours, collects dry particle and is placed in isothermal holding at 110 DEG C
30min, then 900 DEG C are heated to by 5 DEG C/min heating, after 5h is calcined in heat preservation, standing is cooled to room temperature, and grinding distribution crosses 500 mesh
Sieve, obtains binding matrix particle；According to parts by weight, respectively weigh 50 parts of deionized waters, 15 parts of tetrapropylammonium hydroxide, 2 parts receive
Rice silica, 0.2 part of nano-titanium dioxide are placed in three-necked flask, are stirred simultaneously decentralized processing 15min, are obtained reaction solution simultaneously
In mass ratio 1: 25,15% hydrogenperoxide steam generator of mass fraction is added dropwise in reaction solution, control drop rate is 3mL/min,
It after being added dropwise to complete, is stirred and is placed in reaction kettle, in 160 DEG C of reaction kettles for 24 hours with steam crystallization, be centrifugated and receive
Collect lower sediment, rinsed with deionized water to cleaning solution after being in neutrality, then dries at 110 DEG C to constant weight, then at 900 DEG C,
After heat preservation calcining 30min, after standing is cooled to room temperature, matrix desiccant is obtained；According to parts by weight, it is dry that 50 parts of matrixes are weighed respectively
Drying prescription, 5 parts of calcium chloride, 8 parts of microcrystalline celluloses are placed in mortar, and grinding distribution crosses 200 meshes, obtain sieving particle, then press quality
Than 1: 25,20% bromthymol blue ethanol solution of mass fraction is added in sieving particle, is stirred and dries, grounds travel
Broken granulation balling-up can be prepared into the high absorption impervious drying agent for containers material.
Reference examples: the drying agent for containers of Dongguan company production.
The drying agent for containers that example and reference examples are prepared is detected, specific detection is as follows:
Water absorption rate: under the conditions of room temperature (25 DEG C), weighing 0.1g sample and be immersed in 2000mL distilled water, until it is flat to reach swelling
Weighing apparatus.Sample after swelling is filtered separation by filter cloth (500 mesh).Water absorption rate is calculated by formula.
Moisture absorption multiplying power: weighing lg sample and be put into the climatic chamber for setting temperature and humidity, takes out every a period of time,
Survey the hygroscopic capacity of its different time.
Specific test result such as table 1.
1 performance characterization contrast table of table
| Detection project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Reference examples |
| Water absorption rate/g/g | 1894.23 | 1921.05 | 1895.31 | 176.46 |
| Moisture absorption multiplying power/% | 196.6 | 198.3 | 191.2 | 45.4 |
As shown in Table 1, drying agent for containers prepared by the present invention has good moisture pick-up properties.
Claims (9)
1. a kind of preparation method of high absorption impervious drying agent for containers material, it is characterised in that specific preparation step are as follows:
(1) according to parts by weight, 45~50 parts of deionized waters, 10~15 parts of styrene, 3~5 parts of sodium bicarbonates, 6 are weighed respectively
~8 parts of methyl methacrylates and 1~2 part of 1% ammonium persulfate solution of mass fraction are placed in three-necked flask, are stirred and are protected
Temperature reaction, ultrasonic disperse obtain dispersion microsphere lotion；It collects dispersion microsphere lotion and stands isothermal holding in an oven, collect
Dry crystal template；
(2) dry crystal template is added in hydrophobic silicone oil by 1:10 in mass ratio, ramped heating schedule processing, Heat preservation,
Filter and collect filter cake, washing, dry matrix template particles；According to parts by weight, respectively weigh 45~50 parts of dehydrated alcohols,
10~15 parts of 5% magnesium nitrate solutions of mass fraction, 10~15 parts of 5% aluminum nitrate solutions of mass fraction, 3~5 parts of ethyl orthosilicates,
1~2 part of 10% nitric acid of mass fraction and 65~80 parts of deionized waters are placed in conical flask, are stirred and are stood to obtain presoma
Matrix template particles are dipped in precursor solution by solution, stand, filter and collect filter cake, washing, dry, collection drying
Particle and isothermal holding, heating heating, keep the temperature calcination processing, and standing is cooled to room temperature, and grinding distribution sieving obtains binding matrix
Grain；
(3) according to parts by weight, respectively weigh 45~50 parts of deionized waters, 10~15 parts of tetrapropylammonium hydroxide, 1~2 part receive
Rice silica, 0.1~0.2 part of nano-titanium dioxide are placed in three-necked flask, are stirred simultaneously decentralized processing, are obtained reaction solution simultaneously
In mass ratio 1: 25,15% hydrogenperoxide steam generator of mass fraction is added dropwise in reaction solution, after being added dropwise to complete, is stirred simultaneously
It being placed in reaction kettle, Crystallizing treatment, is centrifugated and collects lower sediment, washing, dry, heat preservation calcining remove impurity treatment,
After standing is cooled to room temperature, matrix desiccant is obtained；
(4) according to parts by weight, 45~50 parts of matrix desiccant, 3~5 parts of calcium chloride, 6~8 parts of microcrystalline celluloses are weighed respectively
It is placed in mortar, grinding distribution sieving obtains sieving particle, then in mass ratio 1: 25, by 20% bromthymol blue second of mass fraction
Alcoholic solution is added in sieving particle, is stirred and is dried, grinds granulation balling-up, and the high absorption can be prepared into
Impervious drying agent for containers material.
2. a kind of preparation method of high absorption impervious drying agent for containers material according to claim 1, feature exist
In: in the isothermal holding of standing in an oven oven conditions be humidity be 50%, temperature is 50 DEG C.
3. a kind of preparation method of high absorption impervious drying agent for containers material according to claim 1, feature exist
In: the ramped heating schedule processing is by 3 DEG C/min, and heating is heated to heating at 55~60 DEG C, Heat preservation 2~
3h。
4. a kind of preparation method of high absorption impervious drying agent for containers material according to claim 1, feature exist
In: described dry that matrix template particles are successively to clean 3~5 times with n-hexane, dehydrated alcohol and isopropanol respectively, vacuum
It is freeze-dried to obtain matrix template particles.
5. a kind of preparation method of high absorption impervious drying agent for containers material according to claim 1, feature exist
In: the heating heating, heat preservation calcination processing are heated to 850~900 DEG C by 5 DEG C/min heating, 3~5h of heat preservation calcining.
6. a kind of preparation method of high absorption impervious drying agent for containers material according to claim 1, feature exist
In: the hydrogenperoxide steam generator drop rate is 2~3mL/min.
7. a kind of preparation method of high absorption impervious drying agent for containers material according to claim 1, feature exist
In: the binding matrix grain diameter is 500 mesh.
8. a kind of preparation method of high absorption impervious drying agent for containers material according to claim 1, feature exist
In: the Crystallizing treatment be in 150~160 DEG C of reaction kettles and steam crystallization 20~for 24 hours.
9. a kind of preparation method of high absorption impervious drying agent for containers material according to claim 1, feature exist
In: the heat preservation calcining removal impurity treatment temperature is 850~900 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111001400A (en) * | 2019-12-25 | 2020-04-14 | 华东理工大学 | Titanium dioxide material and preparation method thereof |
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2019
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111001400A (en) * | 2019-12-25 | 2020-04-14 | 华东理工大学 | Titanium dioxide material and preparation method thereof |
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