CN102515237A - Method for preparing nanometer CaCO3 from calcium carbide slag through ultrasonic process - Google Patents
Method for preparing nanometer CaCO3 from calcium carbide slag through ultrasonic process Download PDFInfo
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- CN102515237A CN102515237A CN2011104397581A CN201110439758A CN102515237A CN 102515237 A CN102515237 A CN 102515237A CN 2011104397581 A CN2011104397581 A CN 2011104397581A CN 201110439758 A CN201110439758 A CN 201110439758A CN 102515237 A CN102515237 A CN 102515237A
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Abstract
The invention relates to a method for preparing nanometer CaCO3 from calcium carbide slag through an ultrasonic process. The calcium carbide slag is purified to generate a Ca(OH)2 emulsion, the Ca(OH)2 emulsion which is added with a dispersant, CO2 and air is irradiated by ultrasonic waves, uniformly stirred, suck-filtered and dried to generate the nanometer CaCO3. The method for preparing the nanometer CaCO3 through adopting the ultrasonic process has the advantages of simple operation, no need of designing a new device, high product added value, gas-liquid-solid mass transfer speed improvement benefiting, realization of the resource comprehensive utilization of the industrial waste slag calcium carbide slag, limestone resource consumption reduction, production cost reduction, natural environment improvement, novel technology, operation benefiting, good product stability, substantial shortening of the preparation time, environment improvement, particle size of 30-200nm, and purity of above 99.2%. Production requirements of the rubber industry, the plastic industry and the coating industry are completely met.
Description
Technical field
The present invention relates to the compound technical of International Classification of Patents C01F calcium metal, especially ultrasonic method prepares the method for nano-calcium carbonate with carbide slag.
Background technology
Nano-calcium carbonate production is main material production mostly with the Wingdale in the known technology at present, can consume large quantities of lime stone resource like this, and production cost is high.Prior art is that carborization is with preferred Wingdale high-temperature calcination, obtains quicklime and carbonic acid gas, and quicklime and water reaction then generates refining calcium hydroxide suspension; Logical then people CO
2Gas is used certain tracking monitor means, and behind the reaction terminating, ageing for some time, suction filtration, drying, pulverizing obtain calcium carbonate product.The granularity of lime carbonate and crystal formation are by determining in the carbonization process that the sample quality that carborization obtains is good, and cost is low, are the modal methods of nano-calcium carbonate of producing both at home and abroad at present.
Minimizing along with limestone resource; The production cost of aforementioned technology constantly increases; On the other hand, the industrial residue and the carbide slag environmental pollution that consume after the Wingdale production are but increasing sharply, if can be with the carbide slag of relative low price as raw material replacing lime stone; Its meaning is not just effectively controlled production cost, can also alleviate the environmental pollution that carbide slag causes simultaneously.
The relevant improvement project of less discovery in known technology is raw material like: number of patent application 200510020830 with the carbide slag, adopts chemical precipitation method to prepare the method for calcium carbonate superfine powder.With the exsiccant carbide slag through NH
4Add StNa after removing residue after the dissolving of Cl solution, feed CO again
2Gas, control reaction temperature is at 2～100 ℃.
And for example, number of patent application is 201,010,229,442 1 kinds of methods of utilizing carbide slag to prepare high-purity calcium carbonate superfine, and the method comprising the steps of has: with carbide slag pulverize, sieve, the microwave-assisted heating flame to be to carry out pre-treatment; With concentration be ammonium chloride solution or the ammonium nitrate solution of 1.2～2.0mol/L mix, to leach, followed and filtered filtrating; Add water soluble ion liquid, get mixing solutions; Mixing solutions is mixed with ammonium bicarbonate soln, under microwave irradiation effect, stir, cross and filter the lime carbonate solid; Then with distilled water wash 2～3 times; Place drying under 95～105 ℃ of temperature at last, get powder shaped lime carbonate.
In a word, prior art adopts Wingdale or carbide slag prepares nano-calcium carbonate, complex process; Particle size distribution is wide wayward, and the carburizing reagent time is long, and is difficult to control; Cost is higher, and the product simplification that nano-calcium carbonate manufacturing enterprise produces is functional not strong.
Summary of the invention
The purpose of this invention is to provide a kind of ultrasonic method and prepare the method for nano-calcium carbonate, to reduce production costs, to realize the comprehensive utilization of industrial residue with carbide slag.
Goal of the invention of the present invention realizes through following technical measures: carbide slag generates Ca (OH) through purifying
2Emulsion adds dispersion agent, CO then
2With air Air,, promptly generate nanometer CaCO through suction filtration and drying after restir is even through ultrasonic irradiation
3
The invention has the beneficial effects as follows: adopt ultrasonic method to prepare nano-calcium carbonate, simple to operate, need not design new device, added value of product is high; Help improving the alternate mass transfer velocity of gas, liquid, solid, make the industrial residue carbide slag obtain comprehensive utilization of resources, can reduce the consumption of limestone resource; Reduce production costs, improve physical environment, technology is novel; Be beneficial to operation, product stability is good, and preparation time shortening greatly; Improve environment simultaneously, particle diameter is between 30～200nm, and purity is all more than 99.2%.Meet the requirement of rubber, plastics, coatings industry production fully.
Description of drawings:
Fig. 1 is a technical process simplified schematic diagram of the present invention
Embodiment
Carbide slag generates Ca (OH) through purifying
2Emulsion adds dispersion agent, CO then
2With air Air,, promptly generate nanometer CaCO through suction filtration and drying after restir is even through ultrasonic irradiation
3
Below in conjunction with embodiment, further set forth the present invention.
The industrial residue carbide slag is washed several times with clear water, till sewage change clearly, crossed scalping, remove some mechanical impuritys; Drying is 24 hours under 105 ℃, and cooling is pulverized, and it is 106～250 μ m that carbide slag is ground to particle diameter; Be purified the back carbide slag at 3 hours postcooling of 900 ℃ of temperature lower calcinations, take by weighing the carbide slag after certain mass purifies with electronic analytical balance, with the weight part carbide slag: zero(ppm) water=1: 10 is heated to oil bath pan to 80 ℃ of constant temperature; Put into and fill zero(ppm) water 1000mL beaker, put into magneton then, treat temperature-stable after; Pour carbide slag into beaker, seal with preservative film the beaker top, digests and from oil bath pan, took out beaker in three hours; To obtain calcium hydroxide slurry and filter through 200 mesh sieves, the secluding air storage is subsequent use, places 12 hours; Obtain calcium hydroxide emulsion, earlier with the UW of 40% power, with ultrasonic one hour of postdigestive slurries; And stir simultaneously, in beaker, adding an amount of dispersion agent X 2073, add-on is 0.08% of a carbide slag quality; Then slurries are stirred, with the Ca that stirs (OH)
2Suspension liquid is got 400mL in the 500mL beaker, is poured into then in the 500mL there-necked flask, inserts conductivitimeter and PH meter, opens UW and stirs simultaneously, then bubbling air CO in flask
2Mixed gas, record pH value, specific conductivity and time; Specific conductivity no longer includes noticeable change PH and reduced to 7 o'clock, and carburizing reagent stops, and after the reaction product in the flask is poured in the 500mL flask; Placed two hours, and placed after two hours suction filtration; With zero(ppm) water and each cleaning product of absolute ethyl alcohol three times, product is put into 105 ℃ of loft drier constant temperature, obtain the nanometer grade calcium carbonate product after dry two hours.
The present invention is to use the industrial residue carbide slag, utilizes hyperacoustic energy response and frequency response characteristic, that is to say; This energy and frequency response characteristic are in reaction process, and its phenomenon is pyrolytic decomposition, dissemination and shearing-crushing effect, when in solution, having solid phase to generate; Ultrasonic is different in the cavitation at liquid-solid interface place with effect in neat liquid; Near near solid surface, bubble collapses when going out and can produce local spot erosion and aggravate the effect that particle collides each other solid particle surfaces, and UW is a kind of fluctuation form; Be again a kind of form of energy, it can be accelerated chemical reaction and open up new reaction channel.Lime carbonate through supersound process is carried out the dry final nanometer grade calcium carbonate that obtains of suction filtration.
The nanometer grade calcium carbonate particle diameter that the present invention generates is between 30～200nm, and purity is all more than 99.2%.Meet the requirement of rubber, plastics, coatings industry production fully.
The present invention adopts ultrasonic method to prepare nano-calcium carbonate, and is simple to operate, need not design new device, helps improving the alternate mass transfer velocity of gas, liquid, solid; Do not need additive, technology is novel, and simplicity of design is beneficial to operation; Product stability is good, and preparation time shortening greatly, and cost is lower; Efficient is higher, is convenient to robotization control, helps the large-scale industrial production nano-calcium carbonate.
Claims (3)
1. ultrasonic method prepares the method for nano-calcium carbonate with carbide slag, it is characterized in that: carbide slag generates Ca (OH) through purifying
2Emulsion adds dispersion agent, CO then
2With air Air,, promptly generate nanometer CaCO through suction filtration and drying after restir is even through ultrasonic irradiation
3
2. ultrasonic method as claimed in claim 1 prepares the method for nano-calcium carbonate with carbide slag, it is characterized in that, the industrial residue carbide slag is washed several times with clear water, to sewage become clear till; Cross scalping, remove some mechanical impuritys, 105 ℃ were descended cooling dry 24 hours; Pulverize, it is 106～250 μ m that carbide slag is ground to particle diameter, is purified the back carbide slag at 3 hours postcooling of 900 ℃ of temperature lower calcinations; Take by weighing the carbide slag after certain mass purifies with electronic analytical balance, with the weight part carbide slag: zero(ppm) water=1: 10 is heated to oil bath pan to 80 ℃ of constant temperature; Put into and fill zero(ppm) water 1000mL beaker, put into magneton then, treat temperature-stable after; Pour carbide slag into beaker, seal with preservative film the beaker top, digests and from oil bath pan, took out beaker in three hours; To obtain calcium hydroxide slurry and filter through 200 mesh sieves, the secluding air storage is subsequent use, places 12 hours; Obtain calcium hydroxide emulsion, earlier with the UW of 40% power, with ultrasonic one hour of postdigestive slurries; And stir simultaneously, in beaker, adding an amount of dispersion agent X 2073, add-on is 0.08% of a carbide slag quality; Then slurries are stirred, with the Ca that stirs (OH)
2Suspension liquid is got 400mL in the 500mL beaker, is poured into then in the 500mL there-necked flask, inserts conductivitimeter and PH meter, opens UW and stirs simultaneously, then bubbling air CO in flask
2Mixed gas, record pH value, specific conductivity and time; Specific conductivity no longer includes noticeable change PH and reduced to 7 o'clock, and carburizing reagent stops, and after the reaction product in the flask is poured in the 500mL flask; Placed two hours, and placed after two hours suction filtration; With zero(ppm) water and each cleaning product of absolute ethyl alcohol three times, product is put into 105 ℃ of loft drier constant temperature, obtain the nanometer grade calcium carbonate product after dry two hours.
3. ultrasonic method as claimed in claim 1 prepares the method for nano-calcium carbonate with carbide slag, it is characterized in that the nanometer grade calcium carbonate particle diameter of generation is between 30～200nm, and purity is all more than 99.2%.
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| CN2011104397581A CN102515237A (en) | 2011-12-26 | 2011-12-26 | Method for preparing nanometer CaCO3 from calcium carbide slag through ultrasonic process |
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| CN2011104397581A CN102515237A (en) | 2011-12-26 | 2011-12-26 | Method for preparing nanometer CaCO3 from calcium carbide slag through ultrasonic process |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107902687A (en) * | 2017-12-15 | 2018-04-13 | 柳州吉辉机械设计有限公司 | A kind of method that precipitated calcium carbonate is prepared with gangue |
| CN109231250A (en) * | 2018-12-03 | 2019-01-18 | 衡阳师范学院 | A method of calcining carbide slag prepares calcium carbonate in Galuber's salt type brine cleaning procedure |
| CN109354051A (en) * | 2018-12-03 | 2019-02-19 | 衡阳师范学院 | A method of calcium carbonate is prepared in Galuber's salt type brine cleaning procedure using carbide slag substitution lime |
| CN110577232A (en) * | 2019-10-24 | 2019-12-17 | 长江师范学院 | Preparation method of nano calcium carbonate |
| CN114620727A (en) * | 2022-04-06 | 2022-06-14 | 杨雪兵 | Method for absorbing carbon dioxide in tail gas of cement plant and power plant by using carbide slag |
-
2011
- 2011-12-26 CN CN2011104397581A patent/CN102515237A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 王杰丰: "电石渣超声场下制备纳米碳酸钙研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107902687A (en) * | 2017-12-15 | 2018-04-13 | 柳州吉辉机械设计有限公司 | A kind of method that precipitated calcium carbonate is prepared with gangue |
| CN109231250A (en) * | 2018-12-03 | 2019-01-18 | 衡阳师范学院 | A method of calcining carbide slag prepares calcium carbonate in Galuber's salt type brine cleaning procedure |
| CN109354051A (en) * | 2018-12-03 | 2019-02-19 | 衡阳师范学院 | A method of calcium carbonate is prepared in Galuber's salt type brine cleaning procedure using carbide slag substitution lime |
| CN110577232A (en) * | 2019-10-24 | 2019-12-17 | 长江师范学院 | Preparation method of nano calcium carbonate |
| CN110577232B (en) * | 2019-10-24 | 2022-07-12 | 长江师范学院 | Preparation method of nano calcium carbonate |
| CN114620727A (en) * | 2022-04-06 | 2022-06-14 | 杨雪兵 | Method for absorbing carbon dioxide in tail gas of cement plant and power plant by using carbide slag |
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Application publication date: 20120627 |