CN105329928A - Activation method for nanometer calcium carbonate - Google Patents

Activation method for nanometer calcium carbonate Download PDF

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Publication number
CN105329928A
CN105329928A CN201510909240.8A CN201510909240A CN105329928A CN 105329928 A CN105329928 A CN 105329928A CN 201510909240 A CN201510909240 A CN 201510909240A CN 105329928 A CN105329928 A CN 105329928A
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calcium carbonate
nano
temperature
added
nanometer calcium
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Inventor
阳铁建
谭美蓉
刘小忠
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Hunan Vocational College of Chemical Technology
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Hunan Vocational College of Chemical Technology
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Abstract

The invention provides an activation method for nanometer calcium carbonate. According to the method, normal-temperature fine lime milk with the mass concentration of 10-15% and carbon dioxide are subjected to a full carbonation reaction, the temperature is within the range of 25 DEG C-40 DEG C, and a crystalline-form guiding agent accounting for 0.3-0.5% of the mass of calcium carbonate is added to prepare nanometer calcium carbonate boiled size; the nanometer calcium carbonate boiled size is added into a surface treatment reaction kettle, the stirring speed is 150-300 r/min, a stearic acid absolute ethyl alcohol or palmitic acid chloroform or stearic acid and palmitic acid absolute ethyl alcohol saturated solution with the temperature of 50 DEG C is added to serve as an activating agent, the amount of the solution accounts for 1-2% of the mass of nanometer calcium carbonate dry powder, and stirring continues to be carried out for 30 min; polyacrylamide salt is added to serve as a dispersing agent, the amount of the polyacrylamide salt accounts for 0.5-0.8% of the mass of the nanometer calcium carbonate dry powder, stirring continues to be carried out for 10 min, and the mixture stands for 2 h, and is filtered in a vacuum mode, dried for 2-3 h at the constant temperature of 105 DEG C, ground through a pulverizer and then screened in a 200-mesh mode to obtain a normal-temperature modified nanometer calcium carbonate product. According to the method, normal-temperature activating is achieved, energy loss is reduced, and the requirements for low carbon and environmental protection, resource-conserving and environment-friendly society and sustainable development are met.

Description

A kind of nano-calcium carbonate activation method
Technical field
The present invention relates to technical field of nano material, be specifically related to a kind of nano-calcium carbonate activation method.
Background technology
Wet-process modified is carry out activation treatment to calcium carbonate in ripe slurry solution after carbonization enrichment, utilize calcium carbonate dispersion in the liquid phase more much easier than dispersion in the gas phase, if add dispersion agent, the better feature of dispersion effect, make the effect of calcium carbonate granule and activator molecule evenly.Calcium carbonate granule is after wet-process modified process, and its surface energy reduces, even if form offspring after press filtration, drying, only forms more weak soft-agglomerated of bonding force, efficiently avoid the hard aggregation phenomenon caused because of the generation of chemical bond oxo bridge in dry method modification.To be CN101525146A patent name be publication number " a kind of preparation method of modified nano calcium carbonate " discloses preparation process and be: " 1. in calcium carbonate quality, be reconfigured as the suspension that concentration is 10% ~ 20% after the nano calcium carbonate suspension prepared being filtered; 2. under whipped state, the pH value of suspension, at 70 DEG C ~ 80 DEG C, controls between 6.5 ~ 7.2 by the temperature controlling nano calcium carbonate suspension, drips activator solution, the amount adding activator is 3% ~ 6% of nano-calcium carbonate quality, stirs and is incubated 50 ~ 60 minutes; 3. by the product filtered while hot after above-mentioned process, dry and modified nano calcium carbonate product can be obtained after grinding." wet-process modified there is good coated effect, but ripe for nano-calcium carbonate slurry must be heated to 80 DEG C of activation effects later reaching more satisfactory by wet-process activation usually, and production cost is higher.
Summary of the invention
The technical problem to be solved in the present invention how to make normal temperature wet-process activation arrive more satisfactory activation effect, significantly can reduce again the energy consumption cost of activation.A kind of nano-calcium carbonate activation method of the present invention, in order to solve the problems of the technologies described above, is achieved through the following technical solutions.
A kind of nano-calcium carbonate activation method, step one, obtains calcium oxide by limestone calcination, by calcium oxide and hot water in one to five ratio carry out digestion reaction, then the milk of lime of gained is slightly starched to filter to refine and obtains refined lime breast;
Step 2, the normal temperature refined lime of mass concentration 10-15% breast is carried out abundant carburizing reagent with carbonic acid gas, control the temperature of carbonation reaction within the scope of 25-40 degree by temperature regulating device, and add the crystalline form directed agents of the 0.3-0.5% of calcium carbonate quality, the obtained ripe slurry of nano-calcium carbonate.
Step 3, above-mentioned nano-calcium carbonate slurry is added in surface treatment reaction still, stir speed (S.S.) is that 150-300 turns/min, add the stearic acid dehydrated alcohol of 50 DEG C or palmitinic acid chloroform or stearic acid and palmitinic acid dehydrated alcohol saturated solution as activator, the amount of activator is 1% ~ 2% of nano-calcium carbonate dry powder quality, continues to stir 30min; Then polyacrylamide amine salt is added as dispersion agent, the amount of polyacrylamide amine salt is the nano-calcium carbonate dry powder quality of 0.5% ~ 0.8%, continue to stir 10min, slurries leave standstill 2h, finally adopt vacuum filtration, 105 DEG C of freeze-day with constant temperature 2 ~ 3h, sieve through 200 orders after pulverizing mill grinds, finally obtain normal temperature modified nano-calcium carbonate calcium product.
Crystalline form directed agents is sulfuric acid or inorganic salt.
Compared with activating with traditional intensification, there is following advantage:
1. traditional intensification reactivation process usually adopts and passes into low-pressure steam heating nano-calcium carbonate slurries, and product per ton heats up to activate probably to be needed to consume steam 0.1t, and with steam per ton 200 yuan calculating, the energy consumption cost of light intensification heating is that product per ton reaches 20 yuan.Whole normal temperature activation, reduces the loss of energy, meets the requirement of low-carbon environment-friendly, amphitypy society, Sustainable development.
2. owing to not needing to arrange the heating units such as boiler and equipment, simplify Production Flow Chart, reduce cost of investment and production cost.
Specific embodiment
Embodiment 1
The first step: the normal temperature refined lime of finite concentration 10% breast is carried out carburizing reagent with carbonic acid gas, the temperature 25 degrees Celsius of carbonation reaction is controlled by temperature regulating device, and the sulfuric acid adding 0.1% of calcium carbonate quality does crystalline form directed agents, the obtained ripe slurry of nano-calcium carbonate.
Second step: nano-calcium carbonate slurry is added in surface treatment reaction still, regulate stir speed (S.S.), control to turn/min at 150-300, add activator solution, the amount of activator to be 1% of nano-calcium carbonate dry powder quality the be stearic acid dehydrated alcohol saturated solution of 50 DEG C, continues to stir 30min; Then add dispersion agent, the amount of dispersion agent is 0.5% nano-calcium carbonate dry powder quality, and dispersion agent is polyacrylamide amine salt, continues to stir 10min, and slurries leave standstill 2h.
3rd step: adopt vacuum filtration, 105 DEG C of freeze-day with constant temperature 2 ~ 3h, sieve through 200 orders after pulverizing mill grinds, finally obtain normal temperature modified nano-calcium carbonate calcium product.
Embodiment 2
The first step: the normal temperature refined lime of finite concentration 12% breast is carried out carburizing reagent with carbonic acid gas, the temperature 25 degrees Celsius of carbonation reaction is controlled by temperature regulating device, and the sulfuric acid adding 0.2% of calcium carbonate quality does crystalline form directed agents, the final obtained ripe slurry of nano-calcium carbonate.
Second step: nano-calcium carbonate slurry is added in surface treatment reaction still, regulate stir speed (S.S.), control to turn/min at 150-300, add activator solution, the amount of activator to be 1.2% of nano-calcium carbonate dry powder quality the be stearic acid dehydrated alcohol saturated solution of 50 DEG C, continues to stir 30min; Then add dispersion agent, the amount of dispersion agent is 0.5% nano-calcium carbonate dry powder quality, and dispersion agent is polyacrylamide amine salt, continues to stir 10min, and slurries leave standstill 2h.
3rd step: adopt vacuum filtration, 105 DEG C of freeze-day with constant temperature 2 ~ 3h, sieve through 200 orders after pulverizing mill grinds, finally obtain normal temperature modified nano-calcium carbonate calcium product.
Embodiment 3:
The first step: the normal temperature refined lime of finite concentration 15% breast is carried out carburizing reagent with carbonic acid gas, the temperature 30 degrees Celsius of carbonation reaction is controlled by temperature regulating device, and the sulfuric acid adding 0.3% of calcium carbonate quality does crystalline form directed agents, the final obtained ripe slurry of nano-calcium carbonate.
Second step: nano-calcium carbonate slurry is added in surface treatment reaction still, regulate stir speed (S.S.), control to turn/min at 150-300, add activator solution, the amount of activator to be 1.5% of nano-calcium carbonate dry powder quality the be stearic acid dehydrated alcohol saturated solution of 50 DEG C, continues to stir 30min; Then add dispersion agent, the amount of dispersion agent is 0.5% nano-calcium carbonate dry powder quality, and dispersion agent is polyacrylamide amine salt, continues to stir 10min, and slurries leave standstill 2h.
3rd step: adopt vacuum filtration, 105 DEG C of freeze-day with constant temperature 2 ~ 3h, sieve through 200 orders after pulverizing mill grinds, finally obtain normal temperature modified nano-calcium carbonate calcium product.
Embodiment 4:
The first step: the normal temperature refined lime of finite concentration 12% breast is carried out carburizing reagent with carbonic acid gas, the temperature 30 degrees Celsius of carbonation reaction is controlled by temperature regulating device, and the inorganic salt adding 0.3% of calcium carbonate quality do crystalline form directed agents, the final obtained ripe slurry of nano-calcium carbonate.
Second step: added in surface treatment reaction still by nano-calcium carbonate slurry, regulate stir speed (S.S.), controls to turn/min at 150-300, and the chloroform solvent adding 1% palmitinic acid properties-correcting agent of nano-calcium carbonate dry powder quality fully stirs 30 minutes.Whole modifying process all remains on room temperature.Then add dispersion agent, the amount of dispersion agent is 0.5% nano-calcium carbonate dry powder quality, and dispersion agent is polyacrylamide amine salt, continues to stir 10min, and slurries leave standstill 2h.
3rd step: adopt vacuum filtration, 105 DEG C of freeze-day with constant temperature 2 ~ 3h, sieve through 200 orders after pulverizing mill grinds, finally obtain normal temperature modified nano-calcium carbonate calcium product
Embodiment 5:
The first step: the normal temperature refined lime of finite concentration 12% breast is carried out carburizing reagent with carbonic acid gas, the temperature 30 degrees Celsius of carbonation reaction is controlled by temperature regulating device, and the inorganic salt adding 0.3% of calcium carbonate quality do crystalline form directed agents, the final obtained ripe slurry of nano-calcium carbonate.
Second step: added in surface treatment reaction still by nano-calcium carbonate slurry, regulate stir speed (S.S.), controls to turn/min at 150-300, and the chloroform solvent adding 2% palmitinic acid properties-correcting agent of nano-calcium carbonate dry powder quality fully stirs 30 minutes.Whole modifying process all remains on room temperature.Then add dispersion agent, the amount of dispersion agent is 0.5% nano-calcium carbonate dry powder quality, and dispersion agent is polyacrylamide amine salt, continues to stir 10min, and slurries leave standstill 2h.
3rd step: adopt vacuum filtration, 105 DEG C of freeze-day with constant temperature 2 ~ 3h, sieve through 200 orders after pulverizing mill grinds, finally obtain normal temperature modified nano-calcium carbonate calcium product
Embodiment 6:
The first step: the normal temperature refined lime of finite concentration 12% breast is carried out carburizing reagent with carbonic acid gas, the temperature 30 degrees Celsius of carbonation reaction is controlled by temperature regulating device, and the inorganic salt adding 0.3% of calcium carbonate quality do crystalline form directed agents, the final obtained ripe slurry of nano-calcium carbonate.
Second step: added in surface treatment reaction still by nano-calcium carbonate slurry, regulate stir speed (S.S.), controls to turn/min at 150-300, and the chloroform solvent adding 3% palmitinic acid properties-correcting agent of nano-calcium carbonate dry powder quality fully stirs 30 minutes.Whole modifying process all remains on room temperature.Then add dispersion agent, the amount of dispersion agent is 0.5% nano-calcium carbonate dry powder quality, and dispersion agent is polyacrylamide amine salt, continues to stir 10min, and slurries leave standstill 2h.
3rd step: adopt vacuum filtration, 105 DEG C of freeze-day with constant temperature 2 ~ 3h, sieve through 200 orders after pulverizing mill grinds, finally obtain normal temperature modified nano-calcium carbonate calcium product.
Embodiment 7:
The first step: the normal temperature refined lime of finite concentration 12% breast is carried out carburizing reagent with carbonic acid gas, the temperature 30 degrees Celsius of carbonation reaction is controlled by temperature regulating device, and the inorganic salt adding 0.3% of calcium carbonate quality do crystalline form directed agents, the final obtained ripe slurry of nano-calcium carbonate.
Second step: added in surface treatment reaction still by nano-calcium carbonate slurry, regulate stir speed (S.S.), controls to turn/min at 150-300, adds the dehydrated alcohol properties-correcting agent of the stearic acid of 1% of nano-calcium carbonate dry powder quality, 1% palmitinic acid, fully stirs 30 minutes.Whole modifying process all remains on room temperature.Then add dispersion agent, the amount of dispersion agent is 0.5% nano-calcium carbonate dry powder quality, and dispersion agent is polyacrylamide amine salt, continues to stir 10min, and slurries leave standstill 2h.
3rd step: adopt vacuum filtration, 105 DEG C of freeze-day with constant temperature 2 ~ 3h, sieve through 200 orders after pulverizing mill grinds, finally obtain normal temperature modified nano-calcium carbonate calcium product.
Embodiment 8:
The first step: the normal temperature refined lime of finite concentration 12% breast is carried out carburizing reagent with carbonic acid gas, the temperature 30 degrees Celsius of carbonation reaction is controlled by temperature regulating device, and the inorganic salt adding 0.3% of calcium carbonate quality do crystalline form directed agents, the final obtained ripe slurry of nano-calcium carbonate.
Second step: nano-calcium carbonate slurry is added in surface treatment reaction still, regulate stir speed (S.S.), control to turn/min at 150-300, add the dehydrated alcohol properties-correcting agent of the stearic acid of 1.2% of nano-calcium carbonate dry powder quality, 1.2% palmitinic acid, fully stir 30 minutes.Whole modifying process all remains on room temperature.Then add dispersion agent, the amount of dispersion agent is 0.5% nano-calcium carbonate dry powder quality, and dispersion agent is polyacrylamide amine salt, continues to stir 10min, and slurries leave standstill 2h.
3rd step: adopt vacuum filtration, 105 DEG C of freeze-day with constant temperature 2 ~ 3h, sieve through 200 orders after pulverizing mill grinds, finally obtain normal temperature modified nano-calcium carbonate calcium product.
Embodiment 9:
The first step: the normal temperature refined lime of finite concentration 12% breast is carried out carburizing reagent with carbonic acid gas, the temperature 30 degrees Celsius of carbonation reaction is controlled by temperature regulating device, and the inorganic salt adding 0.3% of calcium carbonate quality do crystalline form directed agents, the final obtained ripe slurry of nano-calcium carbonate.
Second step: nano-calcium carbonate slurry is added in surface treatment reaction still, regulate stir speed (S.S.), control to turn/min at 150-300, add the dehydrated alcohol properties-correcting agent of the stearic acid of 1.5% of nano-calcium carbonate dry powder quality, 1.5% palmitinic acid, fully stir 30 minutes.Whole modifying process all remains on room temperature.Then add dispersion agent, the amount of dispersion agent is 0.5% nano-calcium carbonate dry powder quality, and dispersion agent is polyacrylamide amine salt, continues to stir 10min, and slurries leave standstill 2h.
3rd step: adopt vacuum filtration, 105 DEG C of freeze-day with constant temperature 2 ~ 3h, sieve through 200 orders after pulverizing mill grinds, finally obtain normal temperature modified nano-calcium carbonate calcium product.
The modified nano calcium carbonate product prepared according to above-described embodiment 1-9 after testing activity degree sees the following form 1: detected result shows that the modified nano calcium carbonate Product Activity degree prepared according to the present invention all reaches more than 92%.
Table 1 detected result

Claims (2)

1. a nano-calcium carbonate activation method, is characterized in that:
Step one, obtains calcium oxide by limestone calcination, by calcium oxide and hot water in one to five ratio carry out digestion reaction, then the milk of lime of gained is slightly starched to filter and refiningly obtains refined lime breast;
Step 2, the normal temperature refined lime of mass concentration 10-15% breast is carried out abundant carburizing reagent with carbonic acid gas, control the temperature of carbonation reaction within the scope of 25-40 degree by temperature regulating device, and add the crystalline form directed agents of the 0.1%-0.5% of calcium carbonate quality, the obtained ripe slurry of nano-calcium carbonate;
Step 3, above-mentioned nano-calcium carbonate slurry is added in surface treatment reaction still, stir speed (S.S.) is that 150-300 turns/min, add the stearic acid dehydrated alcohol of 50 DEG C or palmitinic acid chloroform or stearic acid and palmitinic acid dehydrated alcohol saturated solution as activator, the amount of activator is 1% ~ 2% of nano-calcium carbonate dry powder quality, continues to stir 30min; Then polyacrylamide amine salt is added as dispersion agent, the amount of polyacrylamide amine salt is the nano-calcium carbonate dry powder quality of 0.5% ~ 0.8%, continue to stir 10min, slurries leave standstill 2h, finally adopt vacuum filtration, 105 DEG C of freeze-day with constant temperature 2 ~ 3h, sieve through 200 orders after pulverizing mill grinds, finally obtain normal temperature modified nano-calcium carbonate calcium product.
2. a kind of nano-calcium carbonate activation method according to claim 1, described crystalline form directed agents is sulfuric acid or inorganic salt.
CN201510909240.8A 2015-12-10 2015-12-10 Activation method for nanometer calcium carbonate Pending CN105329928A (en)

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CN111056940A (en) * 2019-12-30 2020-04-24 南通新邦化工科技有限公司 Automatic production system and method for calcium stearate
CN111909424A (en) * 2020-07-07 2020-11-10 广西夏阳环保科技有限公司 Preparation method and application of modified nano calcium carbonate for rubber
CN112723402A (en) * 2021-01-11 2021-04-30 广西华纳新材料科技有限公司 Preparation method of monodisperse spindle-shaped precipitated calcium carbonate

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CN111056940A (en) * 2019-12-30 2020-04-24 南通新邦化工科技有限公司 Automatic production system and method for calcium stearate
CN111909424A (en) * 2020-07-07 2020-11-10 广西夏阳环保科技有限公司 Preparation method and application of modified nano calcium carbonate for rubber
CN111909424B (en) * 2020-07-07 2022-06-17 都安春旭新材料科技有限责任公司 Preparation method and application of modified nano calcium carbonate for rubber
CN112723402A (en) * 2021-01-11 2021-04-30 广西华纳新材料科技有限公司 Preparation method of monodisperse spindle-shaped precipitated calcium carbonate
CN112723402B (en) * 2021-01-11 2023-03-31 广西华纳新材料股份有限公司 Preparation method of monodisperse spindle-shaped precipitated calcium carbonate

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Application publication date: 20160217