CN101353486A - Preparation of calcium carbonate complex particle - Google Patents
Preparation of calcium carbonate complex particle Download PDFInfo
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- CN101353486A CN101353486A CNA2008102226505A CN200810222650A CN101353486A CN 101353486 A CN101353486 A CN 101353486A CN A2008102226505 A CNA2008102226505 A CN A2008102226505A CN 200810222650 A CN200810222650 A CN 200810222650A CN 101353486 A CN101353486 A CN 101353486A
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- calcium carbonate
- water glass
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Abstract
The invention discloses a preparation method of calcium carbonate composite particles, comprising the following steps: water glass is added in calcium carbonate pulp with the consistency of 5 percent to 20 percent for mixing; the mixed pulp is heated to 80 to 90 DEG C; reaction is conducted under the stirring condition of 1000r/min to 1500r/min; the reaction time is 0.5 to 1 hour; a PH regulator is added to regulate the PH of the pulp to be 7 to 11; aging is conducted at the temperature of 80 to 90 DEG C after reaction and the aging time is 2 to 5 hours; drying is conducted after aging at the temperature of 120 to 140 DEG C; and the calcium carbonate composite particle is obtained when breaking after drying. The method adopts the PH regulator to better control the PH value change of the solution, can effectively control the SiO2 membrane forming rate to make the SiO2 evenly form membrane on the surface of the calcium carbonate. Water glass is hydrolyzed to form tightly bound hydrated silica layer on the surface of calcium carbonate, having the advantages of simple operation condition, compact structure of made calcium carbonate composite particle and strong acid resistance.
Description
Technical field
The present invention relates to a kind of technology of preparing of calcium carbonate particles, relate in particular to a kind of preparation method that can extensively be used in the conglomerate calcium carbonate composite particles of using as mineral filler etc.
Background technology
Lime carbonate has the starting material source easily, and price is lower, and toxicity is little, and whiteness height, loading level reach the characteristics of mixing good processability greatly, be widely used in the industries such as rubber, coating, papermaking, plastics, and be a kind of important mineral filler.But the lime carbonate surface has very strong polarity, when being applied in those low polar polymkeric substance, need carry out surface modification, to improve the effect of filler-filler and filler-polymkeric substance, is beneficial to the dispersion of lime carbonate in polymeric matrix.Reactive coupling agent commonly used, as silane coupling agent and titanate coupling agent, when being applied to powder and carrying out surface modification, the powder surface active site that should respond.Easy and the lime carbonate effect of titanic acid ester is a little less than silane coupling agent and lime carbonate directly act on.
The treatment process that pair lime carbonate is also arranged in the prior art, these treatment processs have sol-gel method (as the hydrolysis reaction of silicon ester) and chemical precipitation method (as the reaction of water glass with acid).Available technology adopting water glass and sour direct reaction generate sedimentary method, are subjected to the influence of acid, SiO
2Gelling is too fast, understands self nucleation, produces SiO
2Particle then is mixed with SiO in the calcium carbonate granule
2Particle; If gelling is too slow, then SiO
2Be difficult at the calcium carbonate granule surface filming, the lime carbonate surface coats not tight.Adopt the method for the hydrolysis formation sol-gel of silicon ester, exist the treatment time long, precipitate sad filter, difficult dry, need shortcomings such as a large amount of organic solvents.
Summary of the invention
Embodiment of the present invention provides a kind of preparation method of calcium carbonate composite particles, by at surperficial coated Si O
2The mode of film, but a kind of acidproof ability calcium carbonate particles of widespread use by force obtained.
The objective of the invention is to be achieved through the following technical solutions:
Embodiment of the present invention provides a kind of preparation method of calcium carbonate composite particles, and this method comprises:
In concentration is to add water glass in 5%～20% the calcium carbonate serosity to mix, mixed described slurries are heated to 80～90 ℃, under 1000 rev/mins～1500 rev/mins whipped state, react, reaction times is 0.5～1 hour, and adding the pH regulator agent, to regulate the potential of hydrogen of described slurries be 7～11, and the reaction back is 80～90 ℃ of following ageings in temperature, and digestion time is 2～5 hours, carry out drying after the ageing under 120～140 ℃ of temperature, crushed after being dried promptly obtains calcium carbonate composite particles.
Described method also comprises: also add dispersing auxiliary in described calcium carbonate serosity.
Described dispersing auxiliary is any in low-molecular-weight dibasic alcohol, monohydroxy-alcohol, polyethenoxy ether class tensio-active agent, the aluminium salt.
The add-on of described dispersing auxiliary is CaCO in the calcium carbonate serosity
30.1～3% of quality.
Described calcium carbonate serosity and water glass add the potential of hydrogen that described mixed serum is controlled in the pH regulator agent then for adding simultaneously in the reaction vessel.
The pH regulator agent of described adding is any in strong acid, sour gas or the ester class.
The concentration of described calcium carbonate serosity is 5%～20%.
SiO in the water glass solution of described adding
2With CaCO in the described calcium carbonate serosity
3Mass ratio be 5%～25%.
Be 30～120 minutes described time of drying.
The technical scheme that is provided by the invention described above embodiment as can be seen, lime carbonate disperses conditions such as degree, water glass consumption in the potential of hydrogen of embodiment of the present invention by the suitable calcium carbonate serosity concentration of control, slurries, digestion time, the slurries, makes and coats intact SiO
2The calcium carbonate composite particles of film.Make the improved effect of lime carbonate and coupling agent, the lime carbonate surface pH value reduces, the acidproof ability of the calcium carbonate particles that obtains improves, and widens the Application Areas of lime carbonate greatly or strengthens its effect, has simplified the technological process of synthetic calcium carbonate composite particles.This method adopts the pH regulator agent can control the variation of pH value of solution value preferably, controls SiO effectively
2Rate of film build makes SiO
2Equably at the lime carbonate surface filming.Adopt the water glass hydrolysis to form compact hydrated SiO 2 layer on the lime carbonate surface, it is simple that it has operational condition, the calcium carbonate composite particles compact structure of preparation, the advantage that acidproof ability is strong.
Description of drawings
Fig. 1 is the preparation method's of the embodiment of the invention a process flow sheet;
Fig. 2 is the SiO of embodiment of the invention preparation
2/ CaCO
3Mass ratio is the 50000 times of TEM photos of amplification after 20% calcium carbonate composite particles coats.
Fig. 3 is the SiO of embodiment of the invention preparation
2/ CaCO
3Mass ratio is the 100000 times of TEM photos of amplification after 20% calcium carbonate composite particles coats.
Embodiment
Embodiment of the present invention is a kind of preparation method of calcium carbonate composite particles, can prepare the strong calcium carbonate particles of acidproof ability, concrete preparation method comprises: add dispersing auxiliary and mix with water glass in calcium carbonate serosity, under the high degree of agitation, add the pH value that mixed described slurries are regulated in the pH regulator agent, controlled temperature and potential of hydrogen, promptly obtain calcium carbonate composite particles at ageing for some time after the drying.The acidproof ability of this calcium carbonate composite particles is strong, can be applied in a plurality of fields widely.
For ease of understanding, the invention process process is further described below in conjunction with specific embodiments and the drawings.
Embodiment one
Present embodiment provides a kind of preparation method of synthetic calcium carbonate composite particles, can prepare the strong calcium carbonate particles of a kind of acidproof ability, and as shown in Figure 1, concrete preparation method is as follows:
In concentration is 5%～20% calcium carbonate serosity, add water glass solution, SiO in the water glass solution of adding
2With CaCO in this calcium carbonate serosity
3Mass ratio be 5～25%, can also add dispersing auxiliary at calcium carbonate serosity simultaneously, the dispersing auxiliary add-on is 0.1～3% of a described calcium carbonate serosity weight, described mixed slurries are heated to 80～90 ℃, reacted 1～1.5 hour down at high degree of agitation state (referring generally to the whipped state that whipping appts reaches 1000 rev/mins～1500 rev/mins), the pH value that described slurries are regulated in the agent of reaction back adding pH regulator is 8～10, maintain the temperature at 80～90 ℃, ageing is 2～5 hours under constant temperature, carry out washing and filtering after the ageing, carry out drying behind the washing and filtering under 130 ℃ of temperature, be 30～120 minutes time of drying, promptly obtains calcium carbonate composite particles.
Lime carbonate disperses conditions such as degree, water glass consumption in the potential of hydrogen of aforesaid method by the suitable calcium carbonate serosity concentration of control, slurries, digestion time, the slurries, can make and coat intact SiO
2The calcium carbonate composite particles of film.By using sour thinner, simplified the technological process of synthetic calcium carbonate composite particles, and feasible control SiO
2Film formation reaction on the lime carbonate surface is oversimplified, and has except Na
+Outside the ion, bring the advantage of other foreign ion very less into.
This method makes the lime carbonate surface pH value reduce, and the acidproof ability of the calcium carbonate composite particles that makes is improved, and the improved effect of lime carbonate and coupling agent has been widened the Application Areas of lime carbonate greatly, and has also strengthened the effect of lime carbonate.
Embodiment two
Present embodiment provides a kind of preparation method of calcium carbonate composite particles, can prepare the strong calcium carbonate particles of acid resistance ability, uses in the scope that this calcium carbonate composite particles can be wider, and concrete preparation process is as follows:
In concentration is 15% calcium carbonate serosity, add water glass solution, the consumption that adds water glass solution is with the SiO in the water glass solution
2With the CaCO in the described calcium carbonate serosity
3Mass ratio be 15%, described mixed slurries are heated to 85 ℃, under high degree of agitation (state that refers generally to 1000 rev/mins～1500 rev/mins stirs), the pH value that the ethyl acetate that is used as the pH regulator agent is regulated described slurries is 8.5, ageing is 3 hours under 85 ℃ of temperature, carries out washing and filtering, and drying is carried out in the washing back under 130 ℃ temperature, be 60 minutes time of drying, and crushed after being dried promptly obtains calcium carbonate composite particles.
Embodiment three
Present embodiment provides a kind of preparation method of calcium carbonate composite particles, can well prepare the strong calcium carbonate particles of acidproof ability, and concrete preparation process is as follows:
In concentration is 20% calcium carbonate serosity, add water glass solution, the consumption that adds water glass solution is with the SiO in the water glass solution
2With the CaCO in the described calcium carbonate serosity
3Mass ratio be 5%, described mixed slurries are heated to 80 ℃, under high degree of agitation, feed to add CO as the pH regulator agent
2The pH value of regulating described slurries is 9～10, and the constant temperature ageing is 3 hours under 80 ℃ of temperature, carries out washing and filtering, and washing back was 130 ℃ of temperature dryings 50 minutes, and crushed after being dried promptly obtains calcium carbonate composite particles.
Embodiment four
Present embodiment provides a kind of preparation method of calcium carbonate composite particles, can prepare the strong calcium carbonate particles of acidproof ability, and concrete preparation process is as follows:
In concentration is 6% calcium carbonate serosity, add ethylene glycol and water glass solution as dispersing auxiliary, wherein, the add-on of ethylene glycol is for accounting for CaCO in the described calcium carbonate serosity
31% of weight, the consumption that adds water glass solution is with the SiO in the water glass solution
2With the CaCO in the described calcium carbonate serosity
3Mass ratio be 20%, described mixed slurries are heated to 90 ℃, the ethyl acetate adjusting slurry pH value that is used as the pH regulator agent under high degree of agitation is 8.5, ageing is 3 hours under 90 ℃ of temperature, carry out washing and filtering, under 120 ℃ of temperature, carry out drying treatment 100 minutes behind the washing and filtering, promptly obtain calcium carbonate composite particles after the pulverizing.
Embodiment five
Present embodiment provides a kind of preparation method of calcium carbonate composite particles, can prepare the strong calcium carbonate particles of acidproof ability, and concrete preparation process is as follows:
In concentration is 16% calcium carbonate serosity, add Tween80 and water glass solution as dispersing auxiliary, wherein, the add-on of Tween 80 is for accounting for CaCO in the described calcium carbonate serosity
33% of weight, the consumption that adds water glass solution is with the SiO in the water glass solution
2With the CaCO in the described calcium carbonate serosity
3Mass ratio be 25%, heat described mixed slurries to 90 ℃, the dilute sulphuric acid adjusting slurry pH value that is used as the pH regulator agent under high degree of agitation is 8.5, ageing is 3 hours under 90 ℃ of temperature, washing and filtering, under 130 ℃ of temperature, carried out drying 80 minutes behind the washing and filtering, pulverize and promptly obtain calcium carbonate composite particles.
Embodiment six
Present embodiment provides a kind of preparation method of calcium carbonate composite particles, can prepare the strong calcium carbonate particles of acidproof ability, and concrete preparation process is as follows:
In concentration is 10% calcium carbonate serosity, add dispersing auxiliary AlCl
3And water glass solution, slurries are heated to 80 ℃, wherein, AlCl
3Add-on for accounting for CaCO in the described calcium carbonate serosity
32% of weight, the consumption that adds water glass solution is with the SiO in the water glass solution
2With the CaCO in the described calcium carbonate serosity
3Mass ratio be 10%, the ethyl acetate adjusting slurry pH value that is used as the pH regulator agent under high degree of agitation is 8.5, and the constant temperature ageing is 3 hours under 80 ℃ of temperature, carries out washing and filtering, behind the washing and filtering under 140 ℃ of temperature dry 50 minutes, crushed after being dried promptly obtained calcium carbonate composite particles.
Embodiment seven
Present embodiment provides a kind of preparation method of calcium carbonate composite particles, can prepare the strong calcium carbonate particles of a kind of acid resistance ability by this method, and concrete preparation process is as follows:
In concentration is 20% calcium carbonate serosity, add dispersing auxiliary ethylene glycol and water glass solution, heating slurries to 85 ℃, wherein, the add-on of ethylene glycol is for accounting for CaCO in the described calcium carbonate serosity
30.3% of weight, the consumption that adds water glass solution is with the SiO in the water glass solution
2With the CaCO in the described calcium carbonate serosity
3Mass ratio be 5～25%, the pH value that the ethyl acetate that is used as the pH regulator agent under the high degree of agitation is regulated described slurries is 8.5, and the constant temperature ageing is 3 hours under 85 ℃ of temperature, washing and filtering, drying is 120 minutes under 130 ℃ of temperature, and crushed after being dried promptly obtains calcium carbonate composite particles.
Be the raw material detection that experimentizes with the calcium carbonate composite particles for preparing in the foregoing description seven below, specifically check as follows:
The calcium carbonate composite particles that accurately takes by weighing 0.200g preparation is made into 1% the aqueous solution, under high degree of agitation, adds 0.36mol/1HCL, under 25 ℃ of temperature, write down that to keep pH value of solution in 15 minutes be the hydrochloric acid volume of consumption in 5.5 o'clock.The more for a short time calcium carbonate composite particles capacity antacid that shows of salt acid consumption is strong more.
| SiO 2％ | 0 | 5 | 10 | 15 | 20 | 25 |
| Consume hydrochloric acid volume (ml) | 6.50 | 5.40 | 4.42 | 3.55 | 2.45 | 3.60 |
Above-mentioned experimental result shows, with the prepared calcium carbonate composite particles of the embodiment of the invention, keeping pH value of solution in 15 minutes is that the hydrochloric acid volume that consumed in 5.5 o'clock is very little, illustrates that this calcium carbonate composite particles has very strong capacity antacid.
Those skilled in the art by above-mentioned experiment as can be known, and also can predict above-mentioned experiment is the example explanation that experimentizes with the calcium carbonate composite particles of preparation among the embodiment seven only, and the calcium carbonate composite particles (as: calcium carbonate composite particles of preparation among the embodiment two, four, six and seven) that utilizes the preparation method in the embodiment of the invention to prepare all can reach identical effect.
In sum, pass through at surperficial coated Si O in the embodiment of the invention
2Behind the film, make the improved effect of lime carbonate and coupling agent, the lime carbonate surface pH value reduces, and then the acidproof ability raising of the calcium carbonate particles that obtains, thereby has widened the Application Areas of lime carbonate greatly, has also effectively strengthened the effect of calcium carbonate particles.
The above; only be the preferable embodiment of the present invention; but protection scope of the present invention is not limited thereto; protection scope of the present invention is not caused any restriction because of the succession of each embodiment yet; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claim.
Claims (9)
1, a kind of preparation method of calcium carbonate composite particles is characterized in that, this method comprises:
In concentration is to add water glass in 5%～20% the calcium carbonate serosity to mix, mixed described slurries are heated to 80～90 ℃, under 1000 rev/mins～1500 rev/mins whipped state, react, reaction times is 0.5～1 hour, and adding the pH regulator agent, to regulate the potential of hydrogen of described slurries be 7～11, and the reaction back is 80～90 ℃ of following ageings in temperature, and digestion time is 2～5 hours, carry out drying after the ageing under 120～140 ℃ of temperature, crushed after being dried promptly obtains calcium carbonate composite particles.
2, method according to claim 1 is characterized in that, described method also comprises: also add dispersing auxiliary in described calcium carbonate serosity.
3, method according to claim 2 is characterized in that, described dispersing auxiliary is any in low-molecular-weight dibasic alcohol, monohydroxy-alcohol, polyethenoxy ether class tensio-active agent, the aluminium salt.
4, method according to claim 2 is characterized in that, the add-on of described dispersing auxiliary is CaCO in the calcium carbonate serosity
30.1～3% of quality.
5, method according to claim 1 is characterized in that, described calcium carbonate serosity and water glass add the potential of hydrogen that described mixed serum is controlled in the pH regulator agent then for adding simultaneously in the reaction vessel.
According to claim 1 or 3 described methods, it is characterized in that 6, the pH regulator agent of described adding is any in strong acid, sour gas or the ester class.
7, method according to claim 1 is characterized in that, the concentration of described calcium carbonate serosity is 5%～20%.
8, method according to claim 1 is characterized in that, SiO in the water glass solution of described adding
2With CaCO in the described calcium carbonate serosity
3Mass ratio be 5%～25%.
9, method according to claim 1 is characterized in that, be 30～120 minutes described time of drying.
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|---|---|---|---|
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|---|---|---|---|
| CN 200810222650 CN101353486B (en) | 2008-09-19 | 2008-09-19 | Preparation of calcium carbonate complex particle |
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| CN101353486B CN101353486B (en) | 2012-12-12 |
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| CN102020878A (en) * | 2009-09-15 | 2011-04-20 | 上海华明高技术（集团）有限公司 | Method for preparing superfine calcium carbonate compound particles |
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| CN101525260B (en) * | 2009-04-13 | 2012-09-26 | 江西省农业科学院土壤肥料与资源环境研究所 | Special calcium silicon-rich controlled release fertilizer for southern paddy rice and preparation method thereof |
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| US4452262A (en) * | 1981-09-21 | 1984-06-05 | A. W. Faber-Castell | Method of applying cosmetics and medium and device for performing the method |
| CN1167752C (en) * | 2002-04-05 | 2004-09-22 | 中山大学 | Process for preparing nano CaCo3/SiO2 core-shell structure particle |
| CN101225245A (en) * | 2008-01-31 | 2008-07-23 | 上海卓越纳米新材料股份有限公司 | Method for preparing core-shell silicon dioxide coated nano calcium carbonate |
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| CN101525260B (en) * | 2009-04-13 | 2012-09-26 | 江西省农业科学院土壤肥料与资源环境研究所 | Special calcium silicon-rich controlled release fertilizer for southern paddy rice and preparation method thereof |
| CN101565564B (en) * | 2009-06-05 | 2012-04-11 | 石家庄盖尔克斯科技有限公司 | SiO2 enveloped spherical nanometer calcium carbonate and preparation method thereof |
| CN102020878A (en) * | 2009-09-15 | 2011-04-20 | 上海华明高技术（集团）有限公司 | Method for preparing superfine calcium carbonate compound particles |
| CN102020878B (en) * | 2009-09-15 | 2013-05-29 | 上海华明高技术（集团）有限公司 | Method for preparing superfine calcium carbonate compound particles |
| CN102796401A (en) * | 2012-08-17 | 2012-11-28 | 山东宝龙达胶业有限公司 | Preparation method of nanometer calcium carbonate with silica-stearic acid composite coating and special for silicone sealant |
| CN103087352A (en) * | 2013-01-23 | 2013-05-08 | 浙江理工大学 | Method for preparing filling modified material taking CaCO3 as matrix |
| CN103087352B (en) * | 2013-01-23 | 2014-07-16 | 浙江理工大学 | Method for preparing filling modified material taking CaCO3 as matrix |
| CN103131210A (en) * | 2013-02-06 | 2013-06-05 | 浙江工业大学 | Preparation method of composite calcium carbonate |
| CN105671522A (en) * | 2016-01-20 | 2016-06-15 | 东北大学 | Method for coating amorphous silicon dioxide membranes on surfaces of solid particles |
| CN113493209A (en) * | 2020-03-20 | 2021-10-12 | 广州昊吉生物科技有限公司 | Coating method of low-fluorine fluorophlogopite |
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