CN101987926B - Method for preparing nano-level active calcium carbonate for rubber and plastic - Google Patents
Method for preparing nano-level active calcium carbonate for rubber and plastic Download PDFInfo
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- CN101987926B CN101987926B CN 201010257600 CN201010257600A CN101987926B CN 101987926 B CN101987926 B CN 101987926B CN 201010257600 CN201010257600 CN 201010257600 CN 201010257600 A CN201010257600 A CN 201010257600A CN 101987926 B CN101987926 B CN 101987926B
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Abstract
The invention belongs to the technical field of the preparation method of calcium carbonate, and particularly relates to a method for preparing nano-level active calcium carbonate for rubber and plastic. The method comprises the following steps of: a, introducing calcium oxide and water into a paddle-type slaker in proportion, leading a calcium hydroxide suspension into a rough pulp chest after sieving, keeping the slurry standing still in the rough pulp chest and carrying out secondary rotary fluid separation on the rough slurry standing still and then entering a size mixing tank; b, leading the measured calcium hydroxide slurry into a measuring tank for measurement; c, infusing crystallization guiding agent to a carbonizer according to the concentration of the calcium hydroxide slurry, stirring and entering the carbonizer; d, carbonizing in early stage; e, closing carbon dioxide and introducing the slurry in a boiled size tank; f, introducing the slurry in the boiled size tank in a three-level mixed-flow pump after combining by using a metering pump and a surface active agent metering pump, then entering a static-state mixer and finally entering a homogenizing tank; and g, filtering, drying, grinding and screening the slurry in the homogenizing tank. The nano-level active calcium carbonate for rubber and plastic refers to a cubic particle, and has normal appearance and good dispersibility.
Description
Technical field
The present invention relates to calcium carbonate preparation method technical field, especially a kind of method for preparing nano-level active calcium carbonate for rubber.
Background technology
Produce at present nano activated calcium carbonate and generally all adopt carborization, i.e. calcium hydroxide suspension liquid and carbon dioxide reaction generate calcium carbonate, its reaction equation:
Industrialized production is; Band stirs bubbling carborization, multilevel spray carbonization, high-gravity carbonation method.
Carbonization process is calcium carbonate nano particle forming process, and nano-calcium carbonate will have good using value also must carry out surface activation process, i.e. after carbonization finishes, the nano-calcium carbonate slurry is delivered in the surface activation process equipment processes.
Above-mentioned manufacturing technique requirent:
The concentration of calcium hydroxide suspension liquid during carbonization (calcium hydroxide mass percent concentration) is less than 12%, and most of factory adopts below 10%.
Add crystal-directing-agent during carbonization.
Open whipping appts during carbonization.
Carbonization temperature is controlled at below 30 degree Celsius, must cooling move heat.
Carbonization moves to slurry in the surface activation process equipment after finishing, and then slurry is heated to more than 80 degree Celsius, adds prefabricated tensio-active agent, carries out strongly disperseing for a long time and stirring again.
The problem that above-mentioned production technique exists:
Calcium hydroxide concentration is lower during carbonization, so the production intensity of equipment is lower, will throw more fund under identical throughput condition.
Calcium hydroxide concentration is lower during carbonization, and too much mechanical water has increased the energy consumption of heating and cooling meaninglessly.
Carbonization process will stir, and consume electric energy.
Energy expenditure is large, calcium oxide and the water reaction of passing through of calcium hydroxide suspension liquid is produced, and nano-calcium carbonate is produced by calcium hydroxide and carbon dioxide reaction, and these two reactions have a large amount of heat release, want carbonization at low temperature must carry out machinery cooling, the consumption that has brought the energy.
Will be heated to slurry more than 80 degree Celsius during surface activation process, also will award the effect of the high shear force of long-time (about 60 minutes), energy consumption is very large.
Summary of the invention
Produce the very large deficiency of nano activated calcium carbonate energy consumption in order to overcome existing carborization, the invention provides a kind of method for preparing nano-level active calcium carbonate for rubber.
The technical solution adopted for the present invention to solve the technical problems is: a kind of method for preparing nano-level active calcium carbonate for rubber, the method comprises the steps:
A, calcium oxide and water are entered oar formula digestion machine in 1:3.5～5 ratios, the calcium hydroxide suspension liquid enters brown stock chest through 100～200 mesh sieves, slurry was brown stock chest statvolt 24～100 hours, thick slurry through statvolt carries out entering size-mixing tank after the secondary spinning liquid separates, and slurry is interior the allotment to calcium hydroxide mass percent concentration 15～22 of sizing mixing;
B, calcium hydroxide slurry after measured enter the scale tank metering;
C, according to the concentration of calcium hydroxide slurry, inject crystal-directing-agent to carbonating tower, stir and enter carbonating tower after 5～50 minutes;
D, 5～15 minutes carbonization initial stage, the carbonic acid gas inlet is 20～100 cubic meters per minute, then is 5～50 cubic meters per minute, carbonization to 80～90% transfers 5～30 cubic meters per minute to until slurry pH value 6.5～7.0;
E, closing carbon dioxide, slurry enter ripe stock tank;
Slurry in the f, ripe stock tank converges through volume pump and tensio-active agent volume pump and enters three grades of mixedflow pumps, enters motionless mixer again, enters at last balancing reservoir;
Slurry in the g, balancing reservoir carries out press filtration, drying, pulverizing, screening can obtain method for preparing nano-level active calcium carbonate for rubber.
According to another embodiment of the invention, comprise that further described water can be the nano-calcium carbonate factory effluent of tap water or treated mistake.
According to another embodiment of the invention, further comprise described crystal-directing-agent, its consumption is the per-cent 0.05～2 of calcium carbonate quality.
According to another embodiment of the invention, further comprise described tensio-active agent, its consumption is the per-cent 3～7 of calcium carbonate quality.
The invention has the beneficial effects as follows, the present invention compared with prior art, its significant advantage is:
1, broken the conventional art that low-temperature and low-concentration prepares nm-class active calcium carbonate, realized high density normal temperature carbonization, coated and produce nano-calcium carbonate continuously, compare its production technique with conventional art simple, and energy consumption is low.
2, normal temperature coats, and need not heating, saves the energy.
3, employing is coated with continuously and is beneficial to the stable of quality product.
4, the rubber and plastic nanometer grade calcium carbonate of preparation is cubic granules, and pattern is regular, good dispersity.
Description of drawings
The present invention is further described below in conjunction with drawings and Examples.
Fig. 1 is the transmission electron microscope photo;
Fig. 2 coats synoptic diagram continuously.
Among the figure, 1. ripe slurry volume pump, 2. promoting agent volume pump, 3. three grades of mixedflow pumps, 4. motionless mixer, 5. grout outlet.
Embodiment
In conjunction with the accompanying drawings, the present invention is further detailed explanation.These accompanying drawings are the synoptic diagram of simplification, basic structure of the present invention only is described in a schematic way, so it only show the formation relevant with the present invention.
The transmission electron microscope photo such as Fig. 1, a kind of method for preparing nano-level active calcium carbonate for rubber, the method comprises the steps:
A, calcium oxide and water are entered oar formula digestion machine in 1:3.5～5 ratios, the calcium hydroxide suspension liquid enters brown stock chest through 100～200 mesh sieves, slurry was brown stock chest statvolt 24～100 hours, thick slurry through statvolt carries out entering size-mixing tank after the secondary spinning liquid separates, and slurry is interior the allotment to calcium hydroxide mass percent concentration 15～22 of sizing mixing;
B, calcium hydroxide slurry after measured enter the scale tank metering;
C, according to the concentration of calcium hydroxide slurry, inject crystal-directing-agent to carbonating tower, stir and enter carbonating tower after 5～50 minutes;
D, 5～15 minutes carbonization initial stage, the carbonic acid gas inlet is 20～100 cubic meters per minute, then is 5～50 cubic meters per minute, carbonization to 80～90% transfers 5～30 cubic meters per minute to until slurry pH value 6.5～7.0;
E, closing carbon dioxide, slurry enter ripe stock tank;
Slurry in the f, ripe stock tank converges with tensio-active agent volume pump 2 through ripe slurry volume pump 1 and enters three grades of mixedflow pumps 3, enters motionless mixer 4 again, enters balancing reservoir from grout outlet 5 at last; To coat continuously synoptic diagram such as Fig. 2; The acid of tensio-active agent usable resins or lipid acid, soap, oleic acid etc.; Tensio-active agent should cannot not be prefabricated into lowly the liquid of 25% concentration, and the insulation storage enters in the container;
Slurry in the g, balancing reservoir carries out press filtration, drying, pulverizing, screening can obtain method for preparing nano-level active calcium carbonate for rubber.
Described water can be the nano-calcium carbonate factory effluent of tap water or treated mistake.
Described crystal-directing-agent, its consumption are the per-cent 0.05～2 of calcium carbonate quality.
Described tensio-active agent, its consumption are the per-cent 3～7 of calcium carbonate quality.
Embodiment 1:
A kind of method for preparing nano-level active calcium carbonate for rubber, the method comprises the steps:
A, calcium oxide and water are entered oar formula digestion machine in the 1:3.5 ratio, described water can be the nano-calcium carbonate factory effluent of tap water or treated mistake; The calcium hydroxide suspension liquid enters brown stock chest through 120 mesh sieves, and slurry is brown stock chest statvolt 24 hours, carries out entering size-mixing tank after the secondary spinning liquid separates through the thick slurry of statvolt, and slurry is interior the allotment to calcium hydroxide mass percent concentration 15 of sizing mixing;
B, calcium hydroxide slurry after measured enter the scale tank metering;
C, according to the concentration of calcium hydroxide slurry, inject crystal-directing-agent to carbonating tower, described crystal-directing-agent, its amount is to regulate according to the quality index of the finished product and user's requirement, general consumption is the per-cent 0.05 of calcium carbonate quality, stirs and enters carbonating tower after 5 minutes;
D, 5～15 minutes carbonization initial stage, the carbonic acid gas inlet is 20 cubic meters per minute, then is 5 cubic meters per minute, carbonization to 80% transfers 5 cubic meters per minute to until slurry pH value 6.5;
E, closing carbon dioxide, slurry enter ripe stock tank;
Slurry in the f, ripe stock tank converges with tensio-active agent volume pump 2 through ripe slurry volume pump 1 and enters three grades of mixedflow pumps 3, enters motionless mixer 4 again, enters balancing reservoir from grout outlet 5 at last; Described dosage of surfactant is to regulate according to the quality index of the finished product and user's requirement, and general consumption is the per-cent 3 of calcium carbonate quality; The acid of tensio-active agent usable resins or lipid acid, soap, oleic acid etc.; Tensio-active agent should cannot not be prefabricated into lowly the liquid of 25% concentration, and the insulation storage enters in the container;
Slurry in the g, balancing reservoir carries out press filtration, drying, pulverizing, screening can obtain method for preparing nano-level active calcium carbonate for rubber.
Embodiment 2:
A kind of method for preparing nano-level active calcium carbonate for rubber, the method comprises the steps:
A, calcium oxide and water are entered oar formula digestion machine in the 1:4.5 ratio, described water can be the nano-calcium carbonate factory effluent of tap water or treated mistake, the calcium hydroxide suspension liquid enters brown stock chest through 150 mesh sieves, slurry was brown stock chest statvolt 30 hours, thick slurry through statvolt carries out entering size-mixing tank after the secondary spinning liquid separates, and slurry is interior the allotment to calcium hydroxide mass percent concentration 22 of sizing mixing;
B, calcium hydroxide slurry after measured enter the scale tank metering;
C, according to the concentration of calcium hydroxide slurry, inject crystal-directing-agent to carbonating tower, its amount is to regulate according to the quality index of the finished product and user's requirement, general consumption is the per-cent 2 of calcium carbonate quality, stirs and enters carbonating tower after 10 minutes;
D, 5～15 minutes carbonization initial stage, the carbonic acid gas inlet is 40 cubic meters per minute, then is 20 cubic meters per minute, carbonization to 90% transfers 10 cubic meters per minute to until slurry pH value 6.9;
E, closing carbon dioxide, slurry enter ripe stock tank;
Slurry in the f, ripe stock tank converges with tensio-active agent volume pump 2 through ripe slurry volume pump 1 and enters three grades of mixedflow pumps 3, enters motionless mixer 4 again, enters balancing reservoir from grout outlet 5 at last; Described dosage of surfactant is to regulate according to the quality index of the finished product and user's requirement, and general consumption is the per-cent 6 of calcium carbonate quality; The acid of tensio-active agent usable resins or lipid acid, soap, oleic acid etc.; Tensio-active agent should cannot not be prefabricated into lowly the liquid of 25% concentration, and the insulation storage enters in the container;
Slurry in g, the balancing reservoir carries out press filtration, drying, pulverizing, screening etc. and can obtain the coating nanometer grade calcium carbonate.
Embodiment 3:
A kind of method for preparing nano-level active calcium carbonate for rubber, the method comprises the steps:
A, calcium oxide and water are entered oar formula digestion machine in the 1:5 ratio, described water can be the nano-calcium carbonate factory effluent of tap water or treated mistake, the calcium hydroxide suspension liquid enters brown stock chest through 200 mesh sieves, slurry was brown stock chest statvolt 80 hours, thick slurry through statvolt carries out entering size-mixing tank after the secondary spinning liquid separates, and slurry is interior the allotment to calcium hydroxide mass percent concentration 18 of sizing mixing;
B, calcium hydroxide slurry after measured enter the scale tank metering;
C, according to the concentration of calcium hydroxide slurry, inject crystal-directing-agent to carbonating tower, its amount is to regulate according to the quality index of the finished product and user's requirement, general consumption is the per-cent 1.2 of calcium carbonate quality, stirs and enters carbonating tower after 40 minutes;
D, 5～15 minutes carbonization initial stage, the carbonic acid gas inlet is 80 cubic meters per minute, then is 45 cubic meters per minute, carbonization to 88% transfers 25 cubic meters per minute to until slurry pH value 7.0;
E, closing carbon dioxide, slurry enter ripe stock tank;
Slurry in the f, ripe stock tank converges with tensio-active agent volume pump 2 through ripe slurry volume pump 1 and enters three grades of mixedflow pumps 3, enters motionless mixer 4 again, enters balancing reservoir from grout outlet 5 at last; Described dosage of surfactant is to regulate according to the quality index of the finished product and user's requirement, and general consumption is the per-cent 7 of calcium carbonate quality; The acid of tensio-active agent usable resins or lipid acid, soap, oleic acid etc.; Tensio-active agent should cannot not be prefabricated into lowly the liquid of 25% concentration, and the insulation storage enters in the container;
Slurry in g, the balancing reservoir carries out press filtration, drying, pulverizing, screening etc. and can obtain the coating nanometer grade calcium carbonate.
Embodiment 4:
A, employing slurry formula digestion machine can carry out high concentration degradation, and high density is conducive to the abundant digestion of calcium oxide;
B, postdigestive slurry want statvolt more than 24 hours, are convenient to follow-up slurry and purify and modulate;
C, carbonic acid gas volume percent are 20～36;
D, carbonating tower useful volume are 20 cubic metres, and aspect ratio is 7.5:1, and shell will be incubated;
E, carbonating tower carbon dioxide conduit can divide two the tunnel to enter, and can two the road during large flow open simultaneously, can close one the tunnel during normal discharge;
The nucleus that f, variable carbonization mode meet nanometer grade calcium carbonate generates, the rule of growth, also takes full advantage of carbonic acid gas simultaneously;
G, crystal-directing-agent can use sucrose, sulfuric acid, vitriol etc. one or more, can dissolve rear adding;
H, the acid of tensio-active agent usable resins or lipid acid, soap, oleic acid etc.;
I, tensio-active agent should cannot not be prefabricated into lowly the liquid of 25% concentration, and the insulation storage enters in the container;
Operational throughput design and the control of j, ripe slurry and tensio-active agent are to reach by under meter, sequence controller (PLC), frequency transformer.
Take above-mentioned foundation desirable embodiment of the present invention as enlightenment, by above-mentioned description, the relevant staff can in the scope that does not depart from this invention technological thought, carry out various change and modification fully.The technical scope of this invention is not limited to the content on the specification sheets, must determine its technical scope according to the claim scope.
Claims (1)
1. a method for preparing nano-level active calcium carbonate for rubber is characterized in that the method comprises the steps:
A, with calcium oxide and water by mass percentage 1:3.5～5 ratios enter oar formula digestion machine, the calcium hydroxide suspension liquid enters brown stock chest through 100～200 mesh sieves, slurry was brown stock chest statvolt 24～100 hours, thick slurry through statvolt carries out entering size-mixing tank after the secondary spinning liquid separates, and slurry is interior the allotment to calcium hydroxide mass percent concentration 15～22 of sizing mixing;
B, calcium hydroxide slurry after measured enter the scale tank metering;
C, according to the concentration of calcium hydroxide slurry, inject crystal-directing-agent to carbonating tower, stir and enter carbonating tower after 5～50 minutes;
D, 5～15 minutes carbonization initial stages, the carbonic acid gas inlet is 20～100 cubic meters per minute, then is 5～50 cubic meters per minute, carbonization to 80～90%, transfer 5～30 cubic meters per minute to until slurry pH value 6.5～7.0, whole carbonization process carries out at normal temperatures;
E, closing carbon dioxide, slurry enter ripe stock tank;
Slurry in the f, ripe stock tank converges through ripe slurry volume pump (1) and tensio-active agent volume pump (2) and enters three grades of mixedflow pumps (3), enters motionless mixer (4) again, enters balancing reservoir from grout outlet (5) at last;
Slurry in the g, balancing reservoir carries out press filtration, drying, pulverizing, screening can obtain method for preparing nano-level active calcium carbonate for rubber; Wherein, described water is the nano-calcium carbonate factory effluent of tap water or treated mistake; The carbonating tower useful volume is 20 cubic metres, and aspect ratio is 7.5:1, and shell is what be incubated; The carbonating tower carbon dioxide conduit divides two the tunnel to enter, and two the road open simultaneously during large flow, close one the tunnel during normal discharge; Crystal-directing-agent sucrose, sulfuric acid or vitriol; Tensio-active agent is resinous acid, lipid acid or soap; Tensio-active agent cannot not be prefabricated into lowly the liquid of 25% concentration, and the insulation storage enters in the container; Operational throughput design and the control of described ripe slurry and tensio-active agent are to reach by under meter, sequence controller, frequency transformer.
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| CN107129707A (en) * | 2017-05-24 | 2017-09-05 | 福建鸿丰纳米科技有限公司 | The Nano calcium carbonate dedicated preparation method of polysulfide sealant |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1309089A (en) * | 2001-02-16 | 2001-08-22 | 清华大学 | Process for preparing nm-class calcium carbonate |
| CN101456969A (en) * | 2008-12-29 | 2009-06-17 | 南京协和化学有限公司 | Functional calcium carbonate and method for producing the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1309089A (en) * | 2001-02-16 | 2001-08-22 | 清华大学 | Process for preparing nm-class calcium carbonate |
| CN101456969A (en) * | 2008-12-29 | 2009-06-17 | 南京协和化学有限公司 | Functional calcium carbonate and method for producing the same |
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