CN101565198B - Production method of nano calcium carbonate special for organosilicon - Google Patents
Production method of nano calcium carbonate special for organosilicon Download PDFInfo
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- CN101565198B CN101565198B CN2009100992468A CN200910099246A CN101565198B CN 101565198 B CN101565198 B CN 101565198B CN 2009100992468 A CN2009100992468 A CN 2009100992468A CN 200910099246 A CN200910099246 A CN 200910099246A CN 101565198 B CN101565198 B CN 101565198B
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Abstract
The invention relates to a production method of nano calcium carbonate special for organosilicon, comprising the following steps: generating Ca(OH)2 slurry by reacting lime CaO and a proper amount of water, producing the refined raw slurry by a hydraulic cyclone after screening the slurry through a screen cloth; adding a proper amount of crystal form control agent into the modulated raw slurry andplacing the mixture into a carbonization tower after deposition and pumping kiln gas into the carbonization tower to perform carbonization reaction, and pumping the cold water into the carbonizationtower from the bottom of carbonization tower after performing the carbonization reaction for a certain time; placing the boiler slurry into an activation drum and adding the dispersant into the drum and adding saponified surface treating agent into the activation drum after reacting for a certain time; filter pressing, dehydrating, drying and depolymerizing. The depolymerized material is sent to amixer filled with N2 gas and subjected to secondary activating treatment using the coupling agent and crushed and packaged. The production method has features of low production device investment, nano calcium carbonate of composite crystal type, good affinity and harmony with the organosilicon, increased mechanical strength and durability of the downstream products of the organosilicon.
Description
Technical field
The present invention relates to the production method of lime carbonate, mainly is a kind of production method of nano calcium carbonate special for organosilicon.
Background technology
Nano-calcium carbonate is the high-grade calcium carbonate product that grows up at home the nineties in 20th century, because its product quality and performances have all had remarkable improvement than ordinary calcium carbonate, play enhancing, the toughness reinforcing and effect that changes goods processibility, usability in numerous Application Areass, be widely used in fields such as coating, rubber, sizing agent, printing ink, makeup.But domestic nano-calcium carbonate production technology and the exploitation of special application product are all not mature enough, and the production line of producing high-grade nano-calcium carbonate is mainly from external import, and investment of production equipment is more than one hundred million greatly easily, and production cost is higher.
Summary of the invention
The objective of the invention is in order to overcome above-mentioned deficiency, and provide a kind of is the production method of the nano calcium carbonate special for organosilicon of raw material with the calcium oxide, the nano-calcium carbonate of being produced is compound crystal formation, with organosilicon good affinity and blending are arranged, can improve physical strength, the weather resistance of organosilicon downstream product.
The present invention solves the technical scheme that its technical problem adopts: the production method of this nano calcium carbonate special for organosilicon, and step is as follows:
(1), lime CaO and water are by 1: the mass ratio reaction of 6-7 generates Ca (OH)
2Slurries, slurries are made Ca (OH) by 200 eye mesh screens through behind the wet cyclone
2Mass percentage concentration is starched to leave standstill giving birth to of 14-20% and is deposited;
(2), the slurry of giving birth to after will depositing adds water and is modulated into Ca (OH)
2Mass percentage concentration is at 6-7%, and temperature adds and deposits more than half an hour after the crystal formation control agent stirs at 30-35 ℃ slurries, and add-on is mass percent 0.1%-1.0%;
(3), the slurries after will placing squeeze into carbonating tower, feeding concentration is 28-35%, the CO of temperature＜45 ℃
2Carry out carbonization; Squeeze into temperature from the carbonating tower bottom by volume pump when reaction after 20-30 minute and make lime carbonate be compound crystal formation at the cold water below 10 ℃, to slurries PH＜8.0 carburizing reagents end, whole carbon temperature is controlled at below 45 ℃;
(4), the ripe slurry of carbonization gained is squeezed in the activation tube, temperature rises to 75-80 ℃ and adds dispersion agent, and the mass percent of add-on is 0.3%; Add surface treatment agent after 10-20 minute and carry out surface activation process, the mass percent of add-on is 0.25%, after wearing out after activation is finished, and press filtration, oven dry, depolymerization;
(5), depolymerization gained material is sent into fed N
2In the mixing machine of gas, add coupling agent and carry out re-activation, the mass percent of add-on is 0.5%, sieves after crushed, packs.
As preferably, the described crystal formation control agent of step (2) is sucrose, bariumchloride and citric acid, and the mass percent of add-on is respectively 0.1%, 0.4%, 0.4%.
As preferably, be zinc sulfate or Sodium hexametaphosphate 99 at the dispersion agent described in the step (4), surface treatment agent is sodium stearate or lauric acid.
As preferably, be the aluminic acid lipoprotein coupling agent at the coupling agent described in the step (5).
The invention has the advantages that: the nano calcium carbonate special for organosilicon of producing by present method is compound crystal formation (cubes and sheet rectangular parallelepiped), good dispersity, easily oven dry, the product water content is relatively low, with organosilicon good affinity and blending are arranged, can improve physical strength, the weather resistance of organosilicon downstream product.It is low to use the present invention to produce the required technological equipment investment of nano calcium carbonate special for organosilicon, and the product of production use properties in the glue series products of organosilicon downstream is good.The three wastes that produce in the products production, the treated discharging standards that meets.
Embodiment
Below in conjunction with embodiment the present invention is further described, but should understand these embodiment limits the scope of the invention, under the situation of the spirit and scope of the present invention, those skilled in the art can make changes and improvements so that it is fit to different service conditions, condition and embodiment to the present invention.
Embodiment 1:
The production method of this nano calcium carbonate special for organosilicon of the present invention, step is as follows:
(1) lime CaO presses 1 through digestion machine and water: the mass ratio reaction of 6-7 generates Ca (OH)
2Slurries, slurries are made Ca (OH) by 200 eye mesh screens through behind the wet cyclone
2Slurries.Record and give birth to the slurry mass percentage concentration, leave standstill and deposit 17%.
(2) giving birth to after will depositing records Ca (OH) after slurry adds the water modulation
2Mass percentage concentration is 6.5%, and temperature adds crystal formation control agent sucrose, bariumchloride and citric acid at 32 ℃ slurries, and the mass percent of add-on is respectively 0.1%, 0.4%, 0.4%.Deposit 30min.
(3) slurries of taking after the placement are squeezed into carbonating tower, feed kiln gas and carry out carbonization (kiln gas CO
2Concentration 31%, 40 ℃ of temperature).Squeeze into temperature from carbonating tower bottom by volume pump in reaction after 20-30 minute and finish to slurries PH＜8.0 carburizing reagents at 10 ℃ cold water, whole carbon temperature is at 42 ℃.
(4) the ripe slurry of carbonization gained is squeezed in the activation tube, slurry temperature is risen to 75-80 ℃ add dispersion agent zinc sulfate, the mass percent of add-on is 0.3%.Add the surface treatment agent sodium stearate after stirring 15min, the mass percent of add-on is 2.5%.Aging 60min after activation is finished, filter-press dehydration, oven dry, depolymerization.
(5) depolymerization gained material is sent into fed N
2In the mixing machine of gas, add the aluminic acid lipoprotein coupling agent and carry out re-activation, the mass percent of add-on is 0.5%.Taking-up is pulverized, is sieved, packs after mixing 10-15min.Get lime carbonate sample 2000 grams and detect (the results are shown in subordinate list)
Specific embodiment 2:
Dispersion agent among the embodiment 1 is replaced with Sodium hexametaphosphate 99, and surface treatment agent replaces with lauric acid, and other conditions are all identical with example 1.Get lime carbonate sample 2000 grams and detect (the results are shown in subordinate list)
Subordinate list:
| Sequence number | Project | Example 1 | Example 2 |
| 1 | Main content, % | 95.6 | 95.8 |
| 2 | Volatile content below 105 ℃, % | 0.45 | 0.43 |
| 3 | PH value | 9.0 | 9.1 |
| 4 | Hydrochloric acid acid non-soluble substance content, % | 0.01 | 0.01 |
| 5 | Whiteness, degree | 92.5 | 92.0 |
| 6 | Oil-absorption(number), g/100g | 29 | 30 |
| 7 | Specific surface area, m 2/g | 36 | 35 |
| 8 | Degree of activation, % | 98 | 98 |
| 9 | Screenings, 125 μ m | 0.005 | 0.005 |
| 10 | Denseness, cm | 9 | 9 |
In addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection domain of requirement of the present invention.
Claims (3)
1. the production method of a nano calcium carbonate special for organosilicon, it is characterized in that: step is as follows:
(1), lime CaO and water are by 1: the mass ratio reaction of 6-7 generates Ca (OH)
2Slurries, slurries are made Ca (OH) by 200 eye mesh screens through behind the wet cyclone
2Mass percentage concentration is starched to leave standstill giving birth to of 14-20% and is deposited;
(2), the slurry of giving birth to after will depositing adds water and is modulated into Ca (OH)
2Mass percentage concentration is at 6-7%, temperature is at 30-35 ℃ slurries, add and deposit more than half an hour after the crystal formation control agent stirs, add-on is mass percent 0.1%-1.0%, the crystal formation control agent is sucrose, bariumchloride and citric acid, and the mass percent of add-on is respectively 0.1%, 0.4%, 0.4%;
(3), the slurries after will placing squeeze into carbonating tower, feeding concentration is 28-35%, the CO of temperature＜45 ℃
2Carry out carbonization; Squeeze into temperature from the carbonating tower bottom by volume pump when reaction after 20-30 minute and make lime carbonate be compound crystal formation at the cold water below 10 ℃, to slurries pH＜8.0 carburizing reagents end, whole carbon temperature is controlled at below 45 ℃;
(4), the ripe slurry of carbonization gained is squeezed in the activation tube, temperature rises to 75-80 ℃ and adds dispersion agent, and the mass percent of add-on is 0.3%; Add surface treatment agent after 10-20 minute and carry out surface activation process, the mass percent of add-on is 0.25%, after wearing out after activation is finished, and press filtration, oven dry, depolymerization;
(5), depolymerization gained material is sent into fed N
2In the mixing machine of gas, add coupling agent and carry out re-activation, the mass percent of add-on is 0.5%, sieves after crushed, packs.
2. the production method of nano calcium carbonate special for organosilicon according to claim 1, it is characterized in that: at the dispersion agent described in the step (4) is zinc sulfate or Sodium hexametaphosphate 99, and surface treatment agent is sodium stearate or lauric acid.
3. the production method of nano calcium carbonate special for organosilicon according to claim 1, it is characterized in that: at the described coupling agent of step (5) is aluminate coupling agent.
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Cited By (1)
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|---|---|---|---|---|
| US9902652B2 (en) | 2014-04-23 | 2018-02-27 | Calera Corporation | Methods and systems for utilizing carbide lime or slag |
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| CN102732065A (en) * | 2011-04-15 | 2012-10-17 | 池州凯尔特纳米科技有限公司 | Preparation method of PVC special-purpose functional filler superfine active calcium carbonate with low oil absorption |
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| CN105329928A (en) * | 2015-12-10 | 2016-02-17 | 湖南化工职业技术学院 | Activation method for nanometer calcium carbonate |
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| 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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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9902652B2 (en) | 2014-04-23 | 2018-02-27 | Calera Corporation | Methods and systems for utilizing carbide lime or slag |
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