CN103693669A - Method for preparing nano calcium carbonate special for rolling film - Google Patents
Method for preparing nano calcium carbonate special for rolling film Download PDFInfo
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- CN103693669A CN103693669A CN201310642377.2A CN201310642377A CN103693669A CN 103693669 A CN103693669 A CN 103693669A CN 201310642377 A CN201310642377 A CN 201310642377A CN 103693669 A CN103693669 A CN 103693669A
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Abstract
The invention discloses a method for preparing nano calcium carbonate CCR-12 special for a rolling film. The method comprises the steps of calcining limestone used as a raw material to produce quick lime, then subjecting the quick lime to slaking, sieving, ageing to obtain Ca(OH)2 slurry, and carrying out carbonization to realize certain pH value. The method is characterized in that the method comprises the following steps: firstly, taking out and weighing the quick lime produced by the limestone through high-temperature calcination, adding water into the quick lime at a weight ratio of CaO to H2O equal to 1:(5.1-5.5) for slaking, carrying out ageing for 28-32h, sieving, regulating the temperature of the slurry to be at 22-24DEG C, and refining to obtain the Ca(OH)2 slurry with concentration of 11-13%; secondly, blending and refrigerating the Ca(OH)2 slurry, adding a crystal type control agent for reaction when the temperature is regulated to be at 22-24 DEG C, then adding a dispersing agent and introducing CO2 for carbonization, and stopping carbonization until the pH value is equal to 8.4-8.6; thirdly, thickening the carbonized slurry, adding a composite activating agent for activation, and then carrying out dehydration, drying, crushing and grading to obtain nano active calcium carbonate of 80-120nm. The method can achieve good dispersing performance and high blotting capacity of the rolling film.
Description
Technical field
The invention belongs to technical field of inorganic chemical industry, be specially the Nano calcium carbonate dedicated preparation method of calendered film and surface modifying method.
Background technology
Calendered film especially has important effect in China in the Northwest, because rain is little, hair temperature is low, so the Important Action that uses plastic greenhouse to become developing agricultural to produce; In addition it covers in salt pan, the aspect such as industrial packaging, electric insulation, aerated film goods, lamp box advertisement, engineering waterproofing, daily necessities all has a wide range of applications.Calendered film is Nano calcium carbonate dedicated is Nano calcium carbonate dedicated for the particular requirement of calendered film goods, outside meeting the various requirement of calendered film goods, also gives the good dispersing property of calendered film goods and ink receptivity.Nano-calcium carbonate is the mineral filler of a kind of abundant raw material, excellent property, its can part or most of alternative carbon black and white carbon black make the reinforcing filler of silicone adhesive, can reduce costs, there is the features such as the large Bu of loading level Qiang ﹑ whitening effect is good, become gradually the main production raw material of silicone rubber.
Along with Economic development and market in the urgent need to, the water-ground limestone product specific surface area that at present technology is produced is low, crystal formation irregularity, surface modification effect is undesirable, only can be for the production of low-grade hard pipeline.After deliberation, the enhancement of nano-calcium carbonate to calendered film, the factor that affects calendered film product properties is mainly particle form, oil-absorption(number), surface modification and pH value.Therefore in the urgent need to researching and developing a kind of method of the product innovation that can fill for the production of calendered film goods, thoroughly solve the technical problems such as the tensile strength of calendered film goods and elongation is strong not, bad dispersibility, ink receptivity is good not, production stability is poor, to reach the object dominating the market rapidly.
Summary of the invention
For addressing the above problem, the invention provides the Nano calcium carbonate dedicated preparation method of a kind of calendered film and surface modifying method, by controlling crystal formation size and rule degree, from surface modification production technique, set about, realize dispersing property and ink receptivity that calendered film is good.
Technical scheme of the present invention is as follows:
The preparation method that calendered film is Nano calcium carbonate dedicated, take Wingdale as raw material, by making unslaked lime after calcining, through digesting, sieve, after ageing, makes Ca (OH)
2slurries, then reach certain pH value through carbonization, it is characterized in that comprising the steps:
(1) unslaked lime making after Wingdale high-temperature calcination is taken out and weighed, with CaO:H
2o=1:(5.1-5.5) weight ratio adds water by quicklime slaking, after ageing 28-32h, sieves, and regulates the temperature of slurries to 22-24 ℃, is refined into the Ca that concentration is 11-13% (OH)
2slurries;
(2) by Ca (OH)
2raw slurry modulation refrigeration, when temperature is adjusted to 22-24 ℃, adds chemical additives to react, and then adds dispersion agent, logical CO
2carbonization, stops carbonization during to pH=8.4-8.6;
(3) by after the ripe slurry enrichment after carbonization, add composite activating agent activation, after dehydration, dry, pulverizing and classification, obtain the nm-class active calcium carbonate of 80～120nm.
Preferably, in step (3), after dehydration, partial mother liquid is through sedimentation, and the underflow of generation continues cyclic activation.
Preferably, the composition of the described composite activating agent of step (3) is by weight: Oleum Cocois: stearic acid: sodium hydroxide=(78-82): (58-62): (11-15).
Further preferably, the compound method of composite activating agent is: in more than 95 ℃ hot water, by after dissolution of sodium hydroxide, put into stearic acid, guarantee to put Oleum Cocois into after sodium hydroxide and the abundant saponification of stearic acid again.
Preferably, the described high-temperature calcination of step (1) is carried out in shaft kiln or retort furnace, adds coal and air, under the high temperature of 1200 ℃, carries out, and guarantees the raw burn below 6% simultaneously.
Preferably, in step (1), after high-temperature calcination, expellant gas is prepared into highly purified CO after water cooling, purification, compression
2.
Preferably, the described carbonization of step (2) is that to pass into volume fraction be 28～32% CO
2carry out carbonization, the pressure of controlling carbonization system in carbonization process remains on 0.11-0.13MPa, and terminal temperature is controlled at 56-58 ℃.
Preferably, the described chemical additives of step (2) is the zinc sulfate of content 1.8-2.2%.
Preferably, the composition of the described dispersion agent of step (2) is the mixture of refining Oleum Cocois, polyoxyethylene stearic acid ester, alkylphenol polyoxyethylene, polyoxyethylene glycol.
Preferably, the method also comprises the step that reclaims clear liquid and wastewater treatment.
The invention has the beneficial effects as follows:
Adopt the Nano calcium carbonate dedicated preparation method of calendered film of the present invention and surface modifying method, the nano-calcium carbonate specific surface area that makes is moderate, regular crystal forms, surface modification effect are good, can increase substantially good dispersing property and the ink receptivity of calendered film goods.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
By the following examples the specific embodiment of the present invention is further elaborated.
Embodiment 1
Prepare in accordance with the following methods calendered film special-purpose nanometer activated Calcium carbonate CCR-12 of the present invention:
(1) unslaked lime making after Wingdale high-temperature calcination is taken out and weighed, with CaO:H
2the weight ratio of O=1:5.1 adds water by quicklime slaking, after ageing 28h, sieves, and regulates the temperature to 22 ℃ of slurries, is refined into concentration and is 11% Ca (OH)
2slurries;
(2) by Ca (OH)
2raw slurry modulation refrigeration, when temperature is adjusted to 22 ℃, adds chemical additives to react, and then adds dispersion agent, logical CO
2carbonization, stops carbonization during to pH=8.4;
(3) by after the ripe slurry enrichment after carbonization, add composite activating agent activation, after dehydration, dry, pulverizing and classification, obtain the nm-class active calcium carbonate of 80～120nm.
Embodiment 2
Prepare in accordance with the following methods calendered film special-purpose nanometer activated Calcium carbonate CCR-12 of the present invention:
(1) unslaked lime making after Wingdale high-temperature calcination is taken out and weighed, with CaO:H
2the weight ratio of O=1:5.5 adds water by quicklime slaking, after ageing 32h, sieves, and regulates the temperature to 24 ℃ of slurries, is refined into concentration and is 13% Ca (OH)
2slurries;
(2) by Ca (OH)
2raw slurry modulation refrigeration, when temperature is adjusted to 24 ℃, adds chemical additives to react, and then adds dispersion agent, logical CO
2carbonization, stops carbonization during to pH=8.6;
(3) by after the ripe slurry enrichment after carbonization, add composite activating agent activation, after dehydration, dry, pulverizing and classification, obtain the nm-class active calcium carbonate of 80～120nm.
Embodiment 3
Prepare in accordance with the following methods calendered film special-purpose nanometer activated Calcium carbonate CCR-12 of the present invention:
(1) unslaked lime that Wingdale makes after high-temperature calcination takes out and weighs, while hot with CaO:H
2the ratio of O=1:5.3, by quicklime slaking, is sieved after ageing 30h, and its slurry temperature is adjusted to 23 ℃, is refined into concentration and is 12% Ca (OH)
2slurries;
(2) by Ca (OH)
2raw slurry modulation refrigeration, when temperature is adjusted to 23 ℃, adds chemical additives to react, and then adds dispersion agent, logical CO
2carbonization stops carbonization when PH=8.5;
(3) the ripe slurry after carbonization is carried out after enrichment, adding composite activating agent activates, enter immediately Filter Press dehydration, the underflow that partial mother liquid after dehydration produces after sedimentation continues cyclic activation, the warm air that all the other most of wet feeds carry out producing through hotblast stove is dried, and dried powder can make the nm-class active calcium carbonate of 80～120nm after pulverizing, classification.
Embodiment 4
Below with reference to Fig. 1, the preparation method of the Nano calcium carbonate dedicated CCR-12 of calendered film of the present invention and an example of surface modifying method are described.Take Wingdale as raw material, first the Wingdale that the limestone crushing of bulk is become to granularity and be 75～150mm again with the granularity hard coal that is 40～80mm by certain coal blending rate (100:10～100:12), certain interval (3h), certain total amount (being determined by throughput) adds in limestone kiln or retort furnace carries out calcination reaction with air, air is measured (coefficient of excess air is 1.05-1.10) on demand from limestone kiln or retort furnace is sent into (forced ventilation or natural ventilation), the lime generating is by certain interval (3h, match with reinforced, first feed in raw material and go out to obtain afterwards), certain temperature (70-85 ℃) is from bottom, limestone kiln kiln discharge, kiln gas is pressed certain temperature (120～250 ℃) continuously from top, limestone kiln kiln discharge.
From bottom, limestone kiln lime out, digestion machine or digester, carry out digestion reaction (lime is 1:5.3 with the ratio of water) with the hot water from cooling heat exchanger, the concentration of the milk of lime that digestion obtains is about 18%, with cold water, be in harmonious proportion to 13%, first after precipitating thick slag, with three grades of clamor separated with spinning liquid of sieve, refines and ageing 30h again by chute, add chemical additives and water to react, the essence ash breast making will carry out carburizing reagent simultaneously.
From top, limestone kiln kiln gas out, through water Mi washing system, rinse with cooling, temperature is down to after 70～85 ℃, through tar adsorber, purify again, temperature is down to approximately 40 ℃, then enter people's air compressor and compress, from air compressor machine kiln gas out, after oil-gas separator is isolated carried secretly mist of oil, enter the voltage stabilizing of gas-holder buffering, then carry out carburizing reagent with the grey breast of essence, add appropriate dispersion agent simultaneously, produce precipitation of calcium carbonate.
Calcium carbonate suspension after carbonization enters in ripe stock tank, through enrichment, activation, by Filter Press, dehydration, the mother liquor that filtration obtains enters and in settling bowl, carries out gravity settling recovery calcium carbonate wherein, the calcium carbonate reclaiming returns to ripe stock tank, returns to purification together with the clear liquid that the clear liquid of discharging during sedimentation is discharged when enrichment.From pressure filter wet feed (water content≤35%) out, with rotary conveyor, make a gift to someone and after granulation, evenly drop on chain-belt type drying system tablets press and be dried, from moisture eliminator siccative (water content≤0.4%) out after tramp iron separator deironing, make a gift to someone in high speed centrifugation pulverizer and pulverize, from pulverizer powder out, (99.995% crosses 125 μ m sieves, 99.7% crosses 45 μ m sieves, be product calcium carbonate) enter cyclone separation device, the thicker product calcium carbonate of part is sent the fragmentation again that mixes of semifinished product warehouse and virgin material through the bottom of cyclone separation device back to through handling equipment, the thinner product calcium carbonate of qualified part from the top of cyclone separation device out, enter stockyard packing of product warehouse-in.
Embodiment 5
In another embodiment, according to the method for embodiment 4, prepare nano-calcium carbonate CCR-12.In preparation process, in order to be filled into better in organic filler, nano-calcium carbonate is carried out to surface treatment, reach the object of oleophilic drainage.Composite activating agent---Oleum Cocois and stearic acid carry out surface modification treatment in the present embodiment employing, its formula is: Oleum Cocois: stearic acid: sodium hydroxide=80:60:13, unit is kilogram, concrete operation is by after dissolution of sodium hydroxide in more than 95 ℃ hot water, put into stearic acid, guarantee to put again Oleum Cocois into after sodium hydroxide and the abundant saponification of stearic acid, at normal temperatures nano-calcium carbonate is carried out to surface modification, nano-calcium carbonate surface after modification is completely coated, has good dispersing property and ink receptivity.
The present invention is by regulating temperature, the concentration of calcium hydroxide slurry to carry out carbonization, regulate neatly the particle diameter of the calcium carbonate generating, there is higher dispersing property and ink receptivity when making it to be filled into calendered film production technique, adopt compound surface modification treatment agent-Oleum Cocois and stearic acid simultaneously, be filled into better in organic filler, can significantly improve the smooth finish of calendered film goods.
Embodiment 6
The concrete technical parameter of measuring the worth nano-calcium carbonate CCR-12 of embodiment 1-5 the present invention, the results are shown in Table 1:
Table 1
The nano-calcium carbonate specific surface area that makes by the inventive method is moderate, regular crystal forms, surface modification effect are good, can increase substantially good dispersing property and the ink receptivity of calendered film goods.
Claims (10)
1. the Nano calcium carbonate dedicated preparation method of calendered film, take Wingdale as raw material, by making unslaked lime after calcining, through digesting, sieve, after ageing, makes Ca (OH)
2slurries, then reach certain pH value through carbonization, it is characterized in that comprising the steps:
(1) unslaked lime making after Wingdale high-temperature calcination is taken out and weighed, with CaO:H
2o=1:(5.1-5.5) weight ratio adds water by quicklime slaking, after ageing 28-32h, sieves, and regulates the temperature of slurries to 22-24 ℃, is refined into the Ca that concentration is 11-13% (OH)
2slurries;
(2) by Ca (OH)
2raw slurry modulation refrigeration, when temperature is adjusted to 22-24 ℃, adds chemical additives to react, and then adds dispersion agent, logical CO
2carbonization, stops carbonization during to pH=8.4-8.6;
(3) by after the ripe slurry enrichment after carbonization, add composite activating agent activation, after dehydration, dry, pulverizing and classification, obtain the nm-class active calcium carbonate of 80～120nm.
2. the Nano calcium carbonate dedicated preparation method of a kind of calendered film according to claim 1, is characterized in that:
In step (3), after dehydration, partial mother liquid is through sedimentation, and the underflow of generation continues cyclic activation.
3. the Nano calcium carbonate dedicated preparation method of a kind of calendered film according to claim 1, is characterized in that:
The composition of the described composite activating agent of step (3) is by weight: Oleum Cocois: stearic acid: sodium hydroxide=(78-82): (58-62): (11-15).
4. the Nano calcium carbonate dedicated preparation method of a kind of calendered film according to claim 3, is characterized in that:
The compound method of described composite activating agent is: in more than 95 ℃ hot water, by after dissolution of sodium hydroxide, put into stearic acid, guarantee to put Oleum Cocois into after sodium hydroxide and the abundant saponification of stearic acid again.
5. the Nano calcium carbonate dedicated preparation method of a kind of calendered film according to claim 1, is characterized in that:
The described high-temperature calcination of step (1) is carried out in shaft kiln or retort furnace, adds coal and air, under the high temperature of 1200 ℃, carries out, and guarantees the raw burn below 6% simultaneously.
6. the Nano calcium carbonate dedicated preparation method of a kind of calendered film according to claim 1, is characterized in that:
In step (1), after high-temperature calcination, expellant gas is prepared into highly purified CO after water cooling, purification, compression
2.
7. the Nano calcium carbonate dedicated preparation method of a kind of calendered film according to claim 1, is characterized in that:
The described carbonization of step (2) is that to pass into volume fraction be 28～32% CO
2carry out carbonization, the pressure of controlling carbonization system in carbonization process remains on 0.11-0.13MPa, and terminal temperature is controlled at 56-58 ℃.
8. the Nano calcium carbonate dedicated preparation method of a kind of calendered film according to claim 1, is characterized in that:
The described chemical additives of step (2) is the zinc sulfate of content 1.8-2.2%.
9. the Nano calcium carbonate dedicated preparation method of a kind of calendered film according to claim 1, is characterized in that:
The composition of the described dispersion agent of step (2) is the mixture of refining Oleum Cocois, polyoxyethylene stearic acid ester, alkylphenol polyoxyethylene, polyoxyethylene glycol.
10. the Nano calcium carbonate dedicated preparation method of a kind of calendered film according to claim 1, is characterized in that:
Also comprise the step that reclaims clear liquid and wastewater treatment.
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Cited By (13)
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| CN103980733A (en) * | 2014-05-26 | 2014-08-13 | 青州宇信钙业股份有限公司 | Method for synthesizing and modifying highly dispersed nanoscale calcium carbonate and multifunctional calcium carbonate reaction kettle |
| CN104609454A (en) * | 2015-02-11 | 2015-05-13 | 芜湖卓越纳米新材料有限公司 | Method for producing nanometer active calcium carbonate by virtue of cyclic utilization of filtered water |
| CN105400237A (en) * | 2015-12-17 | 2016-03-16 | 广西华纳新材料科技有限公司 | Surface treatment method for nanometer calcium carbonate applied to fill silicone sealant |
| CN105778568A (en) * | 2016-04-18 | 2016-07-20 | 安徽省宣城市华纳新材料科技有限公司 | Surface treatment method for nano calcium carbonate special for photovoltaic adhesive |
| CN107324368A (en) * | 2017-08-10 | 2017-11-07 | 青阳县永诚钙业有限责任公司 | A kind of preparation method of nano-calcium carbonate |
| CN107827138A (en) * | 2017-12-08 | 2018-03-23 | 安徽新涛新材料科技股份有限公司 | A kind of preparation method of superfine active calcium carbonate |
| CN108671895A (en) * | 2018-05-14 | 2018-10-19 | 集美大学 | A kind of more gaps absorption organic volatile nano calcium carbonate composite material and preparation method thereof |
| CN108794810A (en) * | 2018-06-29 | 2018-11-13 | 钦州市宝业坭兴陶厂 | A kind of method of modifying of nano-calcium carbonate and its application in Reinforced PVC tubing |
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| CN111874934A (en) * | 2020-08-14 | 2020-11-03 | 王权广 | Process for preparing regular cubic crystal form nano calcium carbonate |
| CN112250098A (en) * | 2020-10-28 | 2021-01-22 | 衢州顺天钙业有限公司 | High-activity calcium oxide and preparation method thereof |
| CN112811456A (en) * | 2021-01-26 | 2021-05-18 | 江西势通钙业有限公司 | Nano calcium carbonate with high specific surface area and preparation method thereof |
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| CN104609454A (en) * | 2015-02-11 | 2015-05-13 | 芜湖卓越纳米新材料有限公司 | Method for producing nanometer active calcium carbonate by virtue of cyclic utilization of filtered water |
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| CN107324368A (en) * | 2017-08-10 | 2017-11-07 | 青阳县永诚钙业有限责任公司 | A kind of preparation method of nano-calcium carbonate |
| CN107827138A (en) * | 2017-12-08 | 2018-03-23 | 安徽新涛新材料科技股份有限公司 | A kind of preparation method of superfine active calcium carbonate |
| CN108671895A (en) * | 2018-05-14 | 2018-10-19 | 集美大学 | A kind of more gaps absorption organic volatile nano calcium carbonate composite material and preparation method thereof |
| CN108794810A (en) * | 2018-06-29 | 2018-11-13 | 钦州市宝业坭兴陶厂 | A kind of method of modifying of nano-calcium carbonate and its application in Reinforced PVC tubing |
| CN109678697A (en) * | 2018-12-19 | 2019-04-26 | 安徽省宣城市华纳新材料科技有限公司 | A method of recycling fatty acid surface inorganic agent in calcium carbonate production |
| CN110003551A (en) * | 2019-03-29 | 2019-07-12 | 桂林理工大学 | A kind of preparation method of polyethylene hyaline membrane |
| CN111874934A (en) * | 2020-08-14 | 2020-11-03 | 王权广 | Process for preparing regular cubic crystal form nano calcium carbonate |
| CN112250098A (en) * | 2020-10-28 | 2021-01-22 | 衢州顺天钙业有限公司 | High-activity calcium oxide and preparation method thereof |
| CN112811456A (en) * | 2021-01-26 | 2021-05-18 | 江西势通钙业有限公司 | Nano calcium carbonate with high specific surface area and preparation method thereof |
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