CN113247936A - Method for reducing energy consumption in production of nano calcium carbonate - Google Patents
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- C—CHEMISTRY; METALLURGY
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- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/182—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds
- C01F11/183—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds the additive being an organic compound
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Abstract
The invention discloses a method for reducing the production energy consumption of nano calcium carbonate, belonging to the field of nano calcium carbonate preparation, and the method for reducing the production energy consumption of nano calcium carbonate comprises the following steps: s1: adding water to dilute the refined lime milk, adjusting to a suspension with the calcium hydroxide concentration of 7-12%, and adding into a carbonization reactor; s2: adjusting the temperature of the calcium hydroxide suspension to 10-40 ℃, then adding the additive 1 and the additive 2 into the suspension, and uniformly mixing; s3: introducing CO into the suspension2Carbonizing with 10-100 vol% carbonizing gas, introducing gas for 10-30 min when pH of the suspension is reduced to 7.0, and carbonizing to obtain nanometer calcium carbonate suspension at 30-70 deg.C. The invention improves the productivity and the utilization rate of equipment, reduces the production energy consumption, and produces the obtained nano carbonThe calcium carbonate product has high activation degree, low oil absorption value, simple and feasible process, no need of changing the existing process equipment, low production cost and better economic and social benefits.
Description
Technical Field
The invention relates to the field of nano calcium carbonate preparation, in particular to a method for reducing the energy consumption of nano calcium carbonate production.
Background
The nano calcium carbonate is precipitated calcium carbonate with primary particle size within the range of 0-100nm, is applied to the fields of adhesives, printing ink, plastics, rubber, automobile base coats and the like, has obvious functions of strengthening, toughening, regulating and controlling thixotropic property and the like, and is a high-end product in the precipitated calcium carbonate. The calcium carbonate industry in China is the industry with higher energy consumption, and the proportion of energy consumption in the production cost of the nano calcium carbonate is more than 65 percent on average. Therefore, the reduction of the production energy consumption of the nano calcium carbonate has important significance for improving the enterprise competitiveness.
The procedures of the production of the nano calcium carbonate comprise limestone calcination, lime digestion, carbonization, surface treatment, dehydration and drying and the like. At present, the energy conservation and consumption reduction of the production of the nano calcium carbonate mainly reflect the technical upgrading and reconstruction of equipment, for example, the high-efficiency calcining equipment is adopted for calcining limestone to improve the productivity and reduce the energy consumption, a paddle type digesting machine is adopted in a digesting section, a gas distributor is additionally arranged in a carbonizing section, and the like. The equipment upgrading improves the energy consumption problem to a certain extent, but the existing nano calcium carbonate production still adopts the processes of high-temperature digestion, low-temperature carbonization and high-temperature coating, which is an important reason for higher energy consumption of nano calcium carbonate production. Specifically, in the prior art, hot water with the temperature of more than 50 ℃ and calcium oxide are subjected to digestion reaction to obtain calcium hydroxide slurry with the temperature of more than 80 ℃, then the temperature of the calcium hydroxide slurry is reduced to be below 30 ℃, and CO is introduced into the calcium hydroxide slurry2Reacting with calcium hydroxide to generate calcium carbonate, wherein the temperature is 50-60 ℃ after the carbonization reaction, the temperature of calcium carbonate slurry needs to be increased to about 80 ℃ again after the carbonization reaction is finished, and then adding a coating agent such as sodium stearate and the like for surface treatment.
The process of high temperature digestion, low temperature carbonization and high temperature coating is adopted because the supersaturation degree of calcium carbonate nucleation needs to be improved to obtain the nano calcium carbonate, thereby promoting the large-scale nucleation of the calcium carbonate. The supersaturation degree is related to the concentration of calcium ions and carbonate ions in the solution, and the higher the concentration is, the higher the supersaturation degree is, and the easier the nano calcium carbonate is obtained. Solubility of calcium hydroxide in water and CO2The absorption in water is reduced along with the increase of temperature, so the nano calcium carbonate is mostly carbonized at low temperature. After the carbonization is finished, the carbon must be alignedThe rice calcium carbonate is subjected to surface treatment, otherwise the product can be seriously hard agglomerated after being dried and cannot be used. At present, sodium stearate and other treating agents needing high-temperature dissolution are mostly adopted for surface treatment, so that the slurry can obtain better effect only by heating to more than 80 ℃ for coating after carbonization is finished. In addition, in the actual production, in the kiln gas CO2In normal Concentration (CO)2The volume concentration is about 30-35 percent), the carbonization time is more than 10 hours, and the longer carbonization time is also an important reason for increasing the energy consumption of calcium carbonate production.
In order to increase the carbonization reaction rate, Chinese patent CN101723429A discloses a method for utilizing high-concentration CO2The method for producing nano calcium carbonate by using industrial exhaust gas, namely, the method utilizes synthetic ammonia or CO with high concentration discharged by fermentation enterprises2The gas is used as a carbonization gas source to shorten the carbonization reaction time, but most calcium carbonate enterprises have no enterprises around for synthesizing ammonia and the like, so the method has no universal applicability.
Chinese patent CN107488276A discloses a preparation method of high thixotropy nano calcium carbonate, which requires the preparation of kiln gas CO at the initial stage2The concentration is increased to 60-70%, and the nano calcium carbonate suspension is heated to 75-85 ℃ for surface modification after carbonization is finished, and CO is adopted in the method2The enrichment and the surface modification of the nano calcium carbonate suspension greatly increase the energy consumption.
Chinese patent CN110028094A discloses a method for producing active nano calcium carbonate, although CO in kiln gas2The concentration of the calcium carbonate can be controlled to be about 20 percent, but the activation coating temperature of the calcium carbonate slurry is required to be 75-80 ℃, which also accounts for a large proportion of energy consumption.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a method for reducing the energy consumption of nano calcium carbonate production, so as to solve the problems of high energy consumption and no universal applicability in the prior art.
In order to solve the above problems, the present invention adopts the following technical solutions.
A method for reducing the energy consumption of nano calcium carbonate production comprises the following steps:
s1: adding water to dilute the refined lime milk, adjusting to a suspension with the calcium hydroxide concentration of 7-12%, and adding into a carbonization reactor;
s2: adjusting the temperature of the calcium hydroxide suspension to 10-40 ℃, then adding the additive 1 and the additive 2 into the suspension, and uniformly mixing;
s3: introducing CO into the suspension2Carbonizing with 10-100% volume concentration carbonizing gas, introducing gas for 10-30 min when pH of the suspension is reduced to 7.0, and carbonizing to obtain nanometer calcium carbonate suspension at 30-70 deg.C;
s4: adding a surface treating agent into the nano calcium carbonate suspension with the temperature of 30-70 ℃ after the carbonization reaction is finished, stirring for 0.5-2h, and finishing surface modification, wherein the suspension does not need to be heated during modification;
s5: filtering, drying, crushing and depolymerizing the suspension after surface treatment to obtain the nano-scale calcium carbonate product.
As a further description of the above technical solution:
in the step S2, the additive 1 is a nano calcium carbonate crystal form control agent, and the addition amount of the nano calcium carbonate crystal form control agent is 0.1-1.5% of the mass of calcium carbonate.
As a further description of the above technical solution:
in the step S2, the additive 2 is a carbon dioxide absorption enhancer, and the addition amount of the additive 2 is 0.01 per mill to 0.1 percent of the mass of the calcium carbonate, and is preferably 0.02 per mill to 0.05 percent. The addition ratio of less than 0.01 per mill is not obvious in improvement of the carbonization speed, and the addition ratio of more than 0.1% causes obvious increase of the cost and is uneconomical.
As a further description of the above technical solution:
the aeration rate of carbon dioxide during carbonization in the step S3 is 4-24L/(h. mol Ca (OH)2) When the volume flow of the carbon dioxide is lower than 4L/(h.mol Ca (OH)2), the nano calcium carbonate can be obtained, but the reaction time is too long, and the production efficiency is reduced; when the volumetric flow rate of carbon dioxide is higher than 24L/(h. mol. Ca (OH)2), although the reaction is accelerated, aeration equipment is also addedThe load of the air-permeable membrane is high, and the air-permeable rate is too high, so that the problems of poor gel and crystal form development and the like are easily caused.
As a further description of the above technical solution:
in the step S4, the surface treating agent is a water-soluble coating agent, the HLB value of the water-soluble coating agent is more than or equal to 10, the adding proportion of the water-soluble coating agent is 1-6% of the mass of the nano calcium carbonate, and the adding proportion of the water-soluble coating agent is preferably 2-4.5%.
As a further description of the above technical solution:
the processes of filtering, drying, crushing, depolymerizing and the like in the step S5 are consistent with the production of common nano calcium carbonate.
As a further description of the above technical solution:
the nano calcium carbonate crystal form control agent comprises sugar, polyalcohol, hydroxycarboxylic acid and salt thereof, sulfate, inorganic phosphate and other common crystal form control agents in the industry and mixtures thereof, and preferably sucrose, triethanolamine, EDTA and EDTA disodium, zinc sulfate, sodium hexametaphosphate, citric acid and mixtures thereof.
As a further description of the above technical solution:
the carbon dioxide absorption enhancer comprises various surfactants capable of reducing the surface tension of water, and the carbon dioxide absorption enhancer comprises fluorine-containing carbon (-CF)2-，-CF3Etc.) functional group-containing surfactants and silicone surfactants, preferably fluorocarbon (-CF) containing from the viewpoint of use effect2-，-CF3Etc.) functional groups and silicone surfactants because the hydrophobic groups contained in these two classes of surfactants have a superior surface tension reducing effect on water over conventional alkane groups (e.g., -CH)2-，-CH3Etc.). Examples of the fluorine and silicon surfactants include various fluorocarbon surfactants manufactured by DuPont, such as FS520, DR4430, FS22, and FS31, and polyether-modified organosiloxane surfactants such as BYK-346 manufactured by Bick.
As a further description of the above technical solution:
the water-soluble coating agent is preferably one or a mixture of more of sodium oleate, potassium oleate, polyoxyethylene monostearate, polyoxyethylene monolaurate, polyoxyethylene octadecanol and sodium dodecyl sulfate.
Compared with the prior art, the invention has the advantages that:
(1) according to the scheme, the carbonization reaction time of the nano calcium carbonate can be shortened, the productivity and the equipment utilization rate are improved, and the production energy consumption is reduced.
(2) According to the scheme, the low-temperature coating can be realized by adopting the water-soluble coating agent, the coating temperature of the water-soluble coating agent is 30-80 ℃, and heat supply is not needed in the coating process to keep the temperature of the slurry. Can obtain the nano calcium carbonate product with the primary particle size of less than 100nm and various indexes meeting the requirements of GB/T19590-.
(3) The scheme is not only suitable for using normal kiln gas (CO)2Volume concentration of 25% or more) and can be used for producing nano calcium carbonate using low CO2Concentration kiln gas (CO)2Volume concentration of 10-25%) to produce nano calcium carbonate, and can raise low CO content2The carbonization reaction speed of the kiln gas is reduced, and the unit cost is reduced.
(4) The scheme has the advantages of simple and feasible process, no need of changing the existing process equipment, low production cost and better economic and social benefits.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
adding 0.6L of calcium hydroxide suspension with the concentration of 7.5 percent into a carbonization reaction kettle with the volume of 1L;
adjusting the temperature of the suspension to 25 ℃ by a temperature control device, adding 0.3g of sucrose (additive 1) and 0.0012g of surfactant FS31 (additive 2) into the suspension, and uniformly mixing;
introducing mixed gas for carbonization after uniform mixing, wherein the volume flow of carbon dioxide in the mixed gas is 60mL/min, the volume flow of nitrogen is 340mL/min, introducing air for 10min when the pH of the suspension is reduced to 7.0, finishing carbonization reaction after carbonization, and the temperature of the suspension is about 45 ℃ when carbonization is finished;
adding 2.4g of potassium oleate to carry out surface treatment on the nano calcium carbonate suspension for 1 h;
and after the treatment is finished, carrying out suction filtration on the suspension, drying a filter cake in an oven at the temperature of 80 ℃, crushing and depolymerizing to obtain the nano calcium carbonate with the average particle size of about 50nm, wherein the activation degree of a test sample is 100%. About 3.5h was taken from the gas feed until the suspension pH reached 7.0.
Example 2:
adding 0.6L of 11% calcium hydroxide suspension into a carbonization reaction kettle with the volume of 1L;
adjusting the temperature of the suspension to 30 ℃ by a temperature control device, adding 0.9g of zinc sulfate (additive 1) and 0.002g of surfactant BYK-346 (additive 2) into the suspension, and uniformly mixing;
introducing mixed gas for carbonization after uniform mixing, wherein the volume flow of carbon dioxide in the mixed gas is 120mL/min, the volume flow of nitrogen is 240mL/min, introducing air for 10min when the pH value of the suspension is reduced to 7.0, finishing carbonization reaction after carbonization, and the temperature of the suspension is about 55 ℃ when carbonization is finished;
adding 2.4g of polyoxyethylene monostearate to carry out surface treatment on the nano calcium carbonate suspension for 1 h;
and after the treatment is finished, carrying out suction filtration on the suspension, drying a filter cake in an oven at the temperature of 80 ℃, crushing and depolymerizing to obtain the nano calcium carbonate with the average particle size of about 40nm, wherein the activation degree of a test sample is 100%. About 2.4h was taken from the gas feed until the suspension pH reached 7.0.
Example 3:
adding 0.6L of calcium hydroxide suspension with the concentration of 7.5 percent into a carbonization reaction kettle with the volume of 1L;
adjusting the temperature of the suspension to 35 ℃ by a temperature control device, adding a mixture (additive 1) of 0.3g of sucrose and 0.3g of triethanolamine and 0.0018g of surfactant FS520 (additive 2) into the suspension, and uniformly mixing;
introducing mixed gas for carbonization after uniform mixing, wherein the volume flow of carbon dioxide in the mixed gas is 60mL/min, the volume flow of nitrogen is 540mL/min, introducing air for 10min when the pH of the suspension is reduced to 7.0, finishing carbonization reaction after carbonization, and the temperature is about 60 ℃ when carbonization is finished;
adding 2.4g of polyoxyethylene monolaurate to carry out surface treatment on the nano calcium carbonate suspension for 1 h;
and after the treatment is finished, carrying out suction filtration on the suspension, drying a filter cake in an oven at 80 ℃, crushing and depolymerizing to obtain nano calcium carbonate with the average particle size of about 80nm, wherein the activation degree of a test sample is 100%. About 4h was taken from the gas feed until the suspension pH reached 7.0.
Comparative example 1:
this comparative example differs from example 1 in that no additive 2 was added and the remaining reaction conditions were the same as in example 1. As a result, a non-nano-sized precipitated calcium carbonate having an average particle diameter exceeding 100nm was obtained. From the gas feed until the pH of the suspension reached 7.0, the carbonization took about 4.5 hours, which was nearly 30% longer than that of example 1.
It should be noted that the above mentioned processes of filtering, drying, crushing, depolymerizing, etc. are consistent with the production of common nano calcium carbonate, and are not described in detail herein.
The foregoing is only a preferred embodiment of the present invention; the scope of the invention is not limited thereto. Any person skilled in the art should be able to cover the technical scope of the present invention by equivalent or modified solutions and modifications within the technical scope of the present invention.
Claims (10)
1. A method for reducing the energy consumption of nano calcium carbonate production is characterized in that: the method comprises the following steps:
s1: adding water to dilute the refined lime milk, adjusting to a suspension with the calcium hydroxide concentration of 7-12%, and adding into a carbonization reactor;
s2: adjusting the temperature of the calcium hydroxide suspension to 10-40 ℃, then adding the additive 1 and the additive 2 into the suspension, and uniformly mixing;
s3: introducing CO into the suspension2Carbonizing with 10-100% volume concentration carbonizing gas, introducing gas for 10-30 min when pH of the suspension is reduced to 7.0, and carbonizing to obtain nanometer calcium carbonate suspension at 30-70 deg.C;
s4: adding a surface treating agent into the nano calcium carbonate suspension with the temperature of 30-70 ℃ after the carbonization reaction is finished, and stirring for 0.5-2h to complete surface modification;
s5: filtering, drying, crushing and depolymerizing the suspension after surface treatment to obtain the nano-scale calcium carbonate product.
2. The method for reducing the energy consumption of nano calcium carbonate production according to claim 1, wherein the method comprises the following steps: in the step S2, the additive 1 is a nano calcium carbonate crystal form control agent, and the addition amount of the nano calcium carbonate crystal form control agent is 0.1-1.5% of the mass of calcium carbonate.
3. The method for reducing the energy consumption of nano calcium carbonate production according to claim 1, wherein the method comprises the following steps: in the step S2, the additive 2 is a carbon dioxide absorption enhancer, and the addition amount of the additive 2 is 0.01 per mill-0.1% of the mass of the calcium carbonate.
4. The method for reducing the energy consumption of nano calcium carbonate production according to claim 1, wherein the method comprises the following steps: the aeration rate of carbon dioxide during carbonization in the step S3 is 4-24L/(h. mol Ca (OH)2)。
5. The method for reducing the energy consumption of nano calcium carbonate production according to claim 1, wherein the method comprises the following steps: in the step S4, the surface treating agent is a water-soluble coating agent, the HLB value of the water-soluble coating agent is more than or equal to 10, and the adding proportion of the water-soluble coating agent is 1-6% of the mass of the nano calcium carbonate.
6. The method for reducing the energy consumption of nano calcium carbonate production according to claim 2, wherein the method comprises the following steps: the nano calcium carbonate crystal form control agent comprises saccharides, polyols, hydroxycarboxylic acid and salt thereof, sulfate, inorganic phosphate and mixture thereof.
7. The method for reducing the energy consumption of nano calcium carbonate production according to claim 6, wherein the method comprises the following steps: the nano calcium carbonate crystal form control agent comprises sucrose, triethanolamine, EDTA disodium, zinc sulfate, sodium hexametaphosphate, citric acid and a mixture thereof.
8. The method for reducing the energy consumption of nano calcium carbonate production according to claim 3, wherein the method comprises the following steps: the carbon dioxide absorption enhancer includes various types of surfactants capable of reducing the surface tension of water.
9. The method for reducing the energy consumption of nano calcium carbonate production according to claim 8, wherein the method comprises the following steps: the carbon dioxide absorption promoter comprises fluorine-containing carbon (-CF)2-，-CF3Etc.) surface activity of functional groups and silicone surfactants.
10. The method for reducing the energy consumption of nano calcium carbonate production according to claim 5, wherein the method comprises the following steps: the water-soluble coating agent is one or more of sodium oleate, potassium oleate, polyoxyethylene monostearate, polyoxyethylene monolaurate, polyoxyethylene octadecanol and sodium dodecyl sulfate.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114212814A (en) * | 2021-12-16 | 2022-03-22 | 浙江大学 | Preparation method of nano calcium carbonate |
| CN114349036A (en) * | 2021-11-01 | 2022-04-15 | 山东宇信纳米科技有限公司 | Preparation method of nano calcium carbonate for MS glue |
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Cited By (3)
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| CN114349036A (en) * | 2021-11-01 | 2022-04-15 | 山东宇信纳米科技有限公司 | Preparation method of nano calcium carbonate for MS glue |
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| CN114212814A (en) * | 2021-12-16 | 2022-03-22 | 浙江大学 | Preparation method of nano calcium carbonate |
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Application publication date: 20210813 |