CN100542963C - A kind of preparing fiber lightweight calcium - Google Patents

A kind of preparing fiber lightweight calcium Download PDF

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CN100542963C
CN100542963C CNB2006101167233A CN200610116723A CN100542963C CN 100542963 C CN100542963 C CN 100542963C CN B2006101167233 A CNB2006101167233 A CN B2006101167233A CN 200610116723 A CN200610116723 A CN 200610116723A CN 100542963 C CN100542963 C CN 100542963C
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mgco
carbonization
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施晓旦
王彦华
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Yanzhou Mingyang Chemical Co., Ltd.
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Shanghai Dongsheng New Material Co Ltd
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Abstract

The invention discloses a kind of preparing fiber lightweight calcium, it is characterized in that, comprise the steps: needle-like MgCO 3Joining weight concentration is 2-20%Ca (OH) 2Water slurry in, needle-like MgCO 3Add-on be Ca (OH) 2The 0.5-5% of weight (over dry/over dry) feeds then and contains CO 2The gas carbonization, the system temperature during carbonization is 10～90 ℃, CO 2The volumetric concentration of gas is 10-100%, and carbonization carbonization when the pH of system is 6.5-7.5 finishes, and collects product, is fibrous light cakium carbonate; Said needle-like MgCO 3Refer to MgCO 3Length be 1～5 μ m, length-to-diameter ratio is 5～20: 1.Method disclosed by the invention, crystal seed MgCO 3Consumption less, finished product need not wash, and can significantly reduce MgCl 2Consumption, needn't wash with a large amount of water simultaneously in the product follow-up phase, significantly reduce the consumption of water, the minimizing production cost makes product have more competitive power on market.

Description

A kind of preparing fiber lightweight calcium
Technical field
The present invention relates to the preparation method of lime carbonate, relate in particular to a kind of preparing fiber lightweight calcium that plastics strengthen and be used for papermaking filler that is used for.
Background technology
That whisker is meant is complete-dimension single crystal fibre material, because its internal structure is more complete, subsurface defect is less, physical strength is approximately equal to the theoretical strength of interatomic bond power, again because its length-to-diameter ratio is big, comparing not only intensity height with particulate filler, also have the effect that improves the plastics process industrial art performance and improve product surface smooth finish, is the very excellent advanced composite material strengthening and toughening agent of a kind of mechanical property.We are referred to as fiber the whisker that length is long, length-to-diameter ratio is bigger.This fiber is used for papermaking filler and can improves the retention of filler and reduce influence to paper strength.
Lime carbonate is important inorganic chemical product, and particle diameter is generally less than 2 μ m, often makes filler.Be widely used in operations such as rubber, plastics, coating, papermaking and printing ink, ordinary calcium carbonate is raw material usually with the Wingdale, makes unslaked lime through calcining, and unslaked lime adds water digestion and absorbing carbon dioxide carries out carbonization then, and dehydration, drying obtain product at last.
Fibrous light cakium carbonate is meant that length-to-diameter ratio is 20-30, length 20-30 μ m, and the staple fibre of minor axis 0.5-1.0 μ m, the Chang Zuowei filler is used for plastic prod.The fiber light calcium carbonate can also play the effect that improves plastic tensile Young's modulus, bending elastic modulus and resistance to impact shock and improve plastics thermostability and surface smoothness.The fibrous light cakium carbonate raw material sources are extensive, and manufacturing cost is low to be rising type material.
Japanese Patent JP63-256514, JP63-260815 adopt phosphoric acid and soluble phosphate to prepare the method for fibrous light cakium carbonate, but the length of the fibrous light cakium carbonate that obtains is generally less than 10 μ m.Containing aragonite mutually under the condition of lime carbonate crystal seed and described in Japanese Patent JP4-321515, JP4-224110 and the U.S. Pat 5164172, adding phosphoric acid and soluble phosphate prepare the method for fibrous light cakium carbonate, can prepare the fibroid light calcium of length greater than 20 μ m.Described among the Japanese Patent JP2001-354416 and contained Mg 2+High density Ca (OH) 2Feed in the slurry and contain CO 2The gas carbonization obtain aragonite phase fibrous light cakium carbonate, length 10-20 μ m of fibrous light cakium carbonate.Chinese patent CN1641077A also discloses with MgCl 2Be the method for additive preparation fibrous light cakium carbonate, in reaction process, constantly replenish MgCl 2Additive.
The method of above patent disclosure all has certain shortcoming, will use a large amount of additives in the reaction process, increases production cost, a large amount of in addition additives remains in the goods, must totally could use with a large amount of water washings, so just cause technical process long, facility investment is big.
Summary of the invention
The present invention discloses a kind of preparing fiber lightweight calcium, to overcome the above-mentioned defective that prior art exists.
(be called for short fine particle calcium carbonate) preparation method comprises the steps: fibrous light cakium carbonate of the present invention down together
With needle-like MgCO 3Joining weight concentration is 2-20%Ca (OH) 2Water slurry in, Ca (OH) 2The optimum concn of slurry is 5-12%, needle-like MgCO 3Add-on be Ca (OH) 20.5-5% (over dry/over dry) of weight, needle-like MgCO 3Optimal addn be Ca (OH) 21.5-3.5% (over dry/over dry) of weight feeds then and contains CO 2The gas carbonization, the system temperature during carbonization is 10～90 ℃, the optimum temps of the system during carbonization is 30-70 ℃, CO 2The volumetric concentration of gas is 10-100%, and carbonization carbonization when the pH of system is 6.5-7.5 finishes, and collects product, is fibrous light cakium carbonate, and length is 10-80 μ m, and length-to-diameter ratio is 20～80: 1;
Said needle-like MgCO 3Refer to MgCO 3Length be 1～5 μ m, length-to-diameter ratio is 5～20: 1.
Term " over dry " refers to and does not contain moisture content;
Said needle-like MgCO 3Be to prepare like this:
The aqueous solution of solubility magnesium salts and the reactant aqueous solution of alkali are prepared Mg (OH) 2Gel filters, washs Mg (OH) 2Gel is then with Mg (OH) 2Gel adds water, is prepared into weight concentration and is 5-30% water slurry, Mg (OH) 2The optimum weight concentration of gel slurry is 10-20%;
Said solubility magnesium salts is selected from MgCl 2, MgCl 26H 2O, MgSO 4Or MgBr 2In one or more, the solubility magnesium salts preferentially selects anhydrous MgCl 2Or MgCl 26H 2O.
Said alkali is selected from one or more in NaOH, liquid caustic soda, KOH or the ammoniacal liquor, and alkali preferentially selects NaOH or liquid caustic soda, and the volumetric molar concentration of the aqueous solution of alkali is 0.5mol/L～2.0mol/L;
The mol ratio of solubility magnesium salts and alkali is: the solubility magnesium salts: alkali=1: 1～1: 1.2.
With Mg (OH) 2The gel slurry is put into the reactor that has reflux exchanger, adds sodium oxalate in reactor, and the sodium oxalate add-on is equivalent to Mg (OH) 21-50% of oven dry weight, the optimal addn of sodium oxalate are equivalent to Mg (OH) 25-20% of oven dry weight is heated to boiling then, refluxes 5-20 hours, and the optimum reacting time of boiling reflux is 7-12 hours, and collecting reaction product filters, obtains needle-like Mg (OH) 2, washing is then with needle-like Mg (OH) 2Adding water, to be prepared into weight concentration be 1-25% water slurry, needle-like Mg (OH) 2The optimum concn of slurry is 5-15%, and it is 10～100%CO that the slurry feeding contains volumetric concentration 2The gas carbonization, carbonization obtains needle-like MgCO when pH is 6.5-7.5 3, collecting reaction product is said needle-like MgCO 3
Fibroid light calcium of the present invention can be used for the plastics enhancing and is used for papermaking filler, reduces papermaking wood pulp consumption, and minimizing is fallen trees, and helps environment protection.Method disclosed by the invention, crystal seed MgCO 3Consumption less, finished product need not wash, and can significantly reduce MgCl 2Consumption, needn't wash with a large amount of water simultaneously in the product follow-up phase, significantly reduce the consumption of water, the minimizing production cost makes product have more competitive power on market.
Description of drawings
Fig. 1 is the electromicroscopic photograph of the product of embodiment 1.
Fig. 2 is the electromicroscopic photograph of the product of embodiment 6.
Embodiment
Embodiment 1
With 1m 31.0mol/L MgCl 26H 2O solution and 1m 31.2mol/L the NaOH solution reaction be prepared into Mg (OH) 2Gel is with deionized water wash Mg (OH) 2Gel to the filtrate with the AgNO of 1N 3The no white flocs unit of solution check.Then with Mg (OH) 2Gel adds water, and to break into weight concentration be 10% slurry.Add the sodium oxalate of 0.58kg, put into the 1m that condenser is housed then 3Enamel reaction still in, reflux 5 hours obtains needle-like Mg (OH) 2
With needle-like Mg (OH) 2With deionized water filtration, washes clean.Then with needle-like Mg (OH) 2Breaking into weight concentration with deionized water is 5% slurry, feeds that to contain volumetric concentration be 20%CO 2The gas carbonization, carbonization is to obtain needle-like MgCO at 7.1 o'clock to pH 3, with sem observation needle-like MgCO 3Length is 3 μ m, and length-to-diameter ratio is 10:1.With needle-like MgCO 3Slurries filtration obtains solid content 48.0% needle-like MgCO 3Filter cake 173kg.
With above-mentioned needle-like MgCO 3It is 10% Ca (OH) that filter cake 125kg joins 30 tons of weight concentrations 2In the slurry, it is 25%CO that feeding contains volumetric concentration 2The gas carbonization, the temperature during carbonization is 30 ℃, carbonization is that carbonization in 7.1 o'clock finishes to pH, and the fibroid light calcium slurries filtration is obtained 6.51 tons of solid content 62.0% fibroid light calcium filter cakes.With the sem observation staple length is 30 μ m, and length-to-diameter ratio is 20:1.Electromicroscopic photograph is seen Fig. 1.
Embodiment 2
With 1m 31.2mol/L MgCl 2Solution and 1m 31.2mol/L the NaOH solution reaction be prepared into Mg (OH) 2Gel is with deionized water wash Mg (OH) 2Gel to the filtrate with the AgNO of 1N 3The no white flocs unit of solution check.Then with Mg (OH) 2Gel adds water, and to break into weight concentration be 15% slurry.Add the sodium oxalate of 35kg, put into the 1M that condenser is housed then 3Enamel reaction still in, reflux 20 hours obtains needle-like Mg (OH) 2With needle-like Mg (OH) 2With deionized water filtration, washes clean.Then with needle-like Mg (OH) 2Breaking into weight concentration with deionized water is 15% slurry, feeds and contains 10%CO 2The gas carbonization, carbonization is to obtain needle-like MgCO at 7.0 o'clock to pH 3, with sem observation needle-like MgCO 3Length is 5 μ m, and length-to-diameter ratio is 8:1.With needle-like MgCO 3Slurries filtration obtains solid content 51.0% needle-like MgCO 3Filter cake 195kg.
With above-mentioned needle-like MgCO 3Filter cake 30kg joins 15 ton 20% Ca (OH) 2In the slurry, it is 22%CO that feeding contains volumetric concentration 2The gas carbonization, the temperature during carbonization is 50 ℃, carbonization is that carbonization in 7.0 o'clock finishes to pH, and the fibroid light calcium slurries filtration is obtained 6.46 tons of solid content 60.0% fibroid light calcium filter cakes.With the sem observation staple length is 40 μ m, and length-to-diameter ratio is 30:1.
Embodiment 3
With 1m 32.0mol/L MgSO 4Solution and 1m 32.0mol/L the NaOH solution reaction be prepared into Mg (OH) 2Gel is with deionized water wash Mg (OH) 2Gel to the filtrate with the AgNO of 1N 3The no white flocs unit of solution check.Then with Mg (OH) 2Gel adds water, and to break into weight concentration be 25% slurry.The sodium oxalate that adds 23.2kg is put into the enamel reaction still of the 1m3 that condenser is housed then, and reflux 12 hours obtains needle-like Mg (OH) 2With needle-like Mg (OH) 2With deionized water filtration, washes clean.Then with needle-like Mg (OH) 2Breaking into weight concentration with deionized water is 15% slurry, feeds that to contain volumetric concentration be 98%CO 2The gas carbonization, carbonization is to obtain needle-like MgCO at 6.9 o'clock to pH 3, with sem observation needle-like MgCO 3Length is 5 μ m, and length-to-diameter ratio is 15:1.With needle-like MgCO 3Slurries filtration obtains solid content 50.8% needle-like MgCO 3Filter cake 326kg.
With above-mentioned needle-like MgCO 3Filter cake 295kg joins 20 ton 15% Ca (OH) 2In the slurry, it is 27%CO that feeding contains volumetric concentration 2The gas carbonization, the temperature during carbonization is 70 ℃, carbonization is that carbonization in 6.8 o'clock finishes to pH, and the fibroid light calcium slurries filtration is obtained 6.45 tons of solid content 61.0% fibroid light calcium filter cakes.With the sem observation staple length is 50 μ m, and length-to-diameter ratio is 30:1.
Embodiment 4
With 1m 30.9mol/L MgCl 26H 2O solution and 1m 30.9mol/L the NaOH solution reaction be prepared into Mg (OH) 2Gel is with deionized water wash Mg (OH) 2Gel to the filtrate with the AgNO of 1N 3The no white flocs unit of solution check.Then with Mg (OH) 2Gel adds water, and to break into weight concentration be 25% slurry.Add the sodium oxalate of 17.4kg, put into the 1m that condenser is housed then 3Enamel reaction still in, reflux 14 hours obtains needle-like Mg (OH) 2With needle-like Mg (OH) 2With deionized water filtration, washes clean.Then with needle-like Mg (OH) 2Breaking into weight concentration with deionized water is 16% slurry, feeds that to contain volumetric concentration be 14%CO 2The gas carbonization, carbonization is to obtain needle-like MgCO at 6.9 o'clock to pH 3, with sem observation needle-like MgCO 3Length is 3 μ m, and length-to-diameter ratio is 12:1.With needle-like MgCO 3Slurries filtration obtains solid content 49.5% needle-like MgCO 3Filter cake 152kg.
With above-mentioned needle-like MgCO 3Filter cake 79kg joins 17 ton 18% Ca (OH) 2In the slurry, it is 22%CO that feeding contains volumetric concentration 2The gas carbonization, the temperature during carbonization is 10 ℃, carbonization is that carbonization in 7.0 o'clock finishes to pH, and the fibroid light calcium slurries filtration is obtained 6.42 tons of solid content 60.5% fibroid light calcium filter cakes.With the sem observation staple length is 28 μ m, and length-to-diameter ratio is 26:1.
Embodiment 5
With 1m 31.0mol/L MgBr 2Solution and 1m 31.0mol/L the NaOH solution reaction be prepared into Mg (OH) 2Gel is with deionized water wash Mg (OH) 2Gel to the filtrate with the AgNO of 1N 3The no white flocs unit of solution check.Then with Mg (OH) 2Gel adds water, and to break into weight concentration be 26% slurry.Add the sodium oxalate of 3kg, put into the 1m that condenser is housed then 3Enamel reaction still in, reflux 16 hours obtains needle-like Mg (OH) 2With needle-like Mg (OH) 2With deionized water filtration, washes clean.Then with needle-like Mg (OH) 2Breaking into weight concentration with deionized water is 21% slurry, feeds and contains 24%CO 2The gas carbonization, carbonization is to obtain needle-like MgCO at 7.2 o'clock to pH 3, with sem observation needle-like MgCO 3Length is 2.5 μ m, and length-to-diameter ratio is 13:1.With needle-like MgCO 3Slurries filtration obtains solid content 52.0% needle-like MgCO 3Filter cake 160kg.
With above-mentioned needle-like MgCO 3Filter cake 104kg joins 18 ton 17% Ca (OH) 2In the slurry, it is 23%CO that feeding contains volumetric concentration 2The gas carbonization, the temperature during carbonization is 70 ℃, carbonization is that carbonization in 7.2 o'clock finishes to pH, and the fibroid light calcium slurries filtration is obtained 6.18 tons of solid content 62.8% fibroid light calcium filter cakes.With the sem observation staple length is 18 μ m, and length-to-diameter ratio is 70:1.
Embodiment 6
With 1m 30.5mol/L MgCl 2Solution and 1m 30.5mol/L the NaOH solution reaction be prepared into Mg (OH) 2Gel is with deionized water wash Mg (OH) 2Gel to the filtrate with the AgNO of 1N 3The no white flocs unit of solution check.Then with Mg (OH) 2Gel adds water, and to break into weight concentration be 6% slurry.Add the sodium oxalate of 1.1kg, put into the 1m that condenser is housed then 3Enamel reaction still in, reflux 9 hours obtains needle-like Mg (OH) 2With needle-like Mg (OH) 2With deionized water filtration, washes clean.Then with needle-like Mg (OH) 2Breaking into weight concentration with deionized water is 23% slurry, feeds that to contain volumetric concentration be 12%CO 2The gas carbonization, carbonization is to obtain needle-like MgCO at 6.8 o'clock to pH 3, with sem observation needle-like MgCO 3Length is 1 μ m, and length-to-diameter ratio is 6:1.With needle-like MgCO 3Slurries filtration obtains solid content 48.2% needle-like MgCO 3Filter cake 87kg.
With above-mentioned needle-like MgCO 3Filter cake 22kg joins 30 ton 2% Ca (OH) 2In the slurry, it is 28%CO that feeding contains volumetric concentration 2The gas carbonization, the temperature during carbonization is 60 ℃, carbonization is that carbonization in 6.6 o'clock finishes to pH, and the fibroid light calcium slurries filtration is obtained 1.27 tons of solid content 61.3% fibroid light calcium filter cakes.With the sem observation staple length is 40 μ m, and length-to-diameter ratio is 34:1.Electromicroscopic photograph is seen Fig. 2.
Embodiment 7
The fibroid light calcium of embodiment 6 preparation and common fine particle calcium carbonate are applied to the simultaneous test of papermaking by different ratios, and the median size of common fine particle calcium carbonate is 1.5 μ m.Slurry: broad-leaved slurry (25 0SR): needle slurry (45 0SR)=and 60:40 (weight), after slurry mixes, beating degree 35.6 0SR.Experimentation: oven dry stock is pressed 70g/m 2Constant, the dosage of filler is respectively 15%, 20%, 25%, 30%, 40% (over dry/oven dry stock), take by weighing an amount of slurry, stir after 1 minute, adding filler stirred 1 minute, square copying copied the sheet shaping on the sheet machine in the laboratory, and drying, 0.3Mpa soft calendaring detect pattern intensity, ash index.Press GB/T453-2002 and detect pattern intensity.
Figure C200610116723D00081
Embodiment 8
Use the dynamic drainage instrument and investigate fibroid light calcium reservation situation: slurry: broad-leaved slurry (25 0SR): needle slurry (45 0SR)=and 60:40 (weight), after slurry mixes, beating degree 35.6 0SR.Design after 5 seconds, is pressed load weighted paper pulp stirring respectively different process adding filler and was stirred 5 seconds by online concentration 0.6% (weight), gets machine water 100ml, detectable level, ash, parallel laboratory test 2 times.The median size of common fine particle calcium carbonate is 1.5 μ m, and the median size of water-ground limestone is 1.0 μ m.Detected result such as following table:
The method of calculation of test-results:
White water consistency=(÷ of poor quality 100 before and after the filter paper) * 100%
Total retention rate=[(online concentration-white water consistency) ÷ surf the Net concentration] * 100%
Weight ÷ plain boiled water filter residue quality after plain boiled water filter residue ash=plain boiled water filter residue calcination
Fiber retention rate=(design fiber add-on-fibre stream vector) ÷ design fiber add-on
Filler retention=(design filling adding amount-plain boiled water ash) ÷ designs filling adding amount.
Figure C200610116723D00091

Claims (8)

1. a preparing fiber lightweight calcium is characterized in that, comprises the steps: needle-like MgCO 3Joining weight concentration is 2-20%Ca (OH) 2Water slurry in, the needle-like MgCO of adding 3Weight is with respect to Ca (OH) 2Weight counts 0.5-5% with over dry/over dry, feeds then and contains CO 2The gas carbonization, the system temperature during carbonization is 10～90 ℃, CO 2The volumetric concentration of gas is 10-100%, and carbonization carbonization when the pH of system is 6.5-7.5 finishes, and collects product, is fibrous light cakium carbonate;
Said needle-like MgCO 3Refer to MgCO 3Length be 1～5 μ m, length-to-diameter ratio is 5～20: 1.
2. method according to claim 1 is characterized in that, said needle-like MgCO 3Be to prepare like this:
The aqueous solution of solubility magnesium salts and the reactant aqueous solution of alkali are prepared Mg (OH) 2Gel filters, washs Mg (OH) 2Gel is then with Mg (OH) 2Gel adds water, is prepared into weight concentration and is 5-30% water slurry;
With Mg (OH) 2The gel slurry is put into the reactor that has reflux exchanger, adds sodium oxalate in reactor, and the sodium oxalate add-on is equivalent to Mg (OH) 21-50% of oven dry weight is heated to boiling then, refluxes 5-20 hours, and the reaction times of boiling reflux is 7-12 hours, and collecting reaction product filters, obtains needle-like Mg (OH) 2, washing is then with needle-like Mg (OH) 2Adding water, to be prepared into weight concentration be 1-25% water slurry, and slurry feeds that to contain volumetric concentration be 10～100%CO 2The gas carbonization, carbonization obtains needle-like MgCO when pH is 6.5-7.5 3, collecting reaction product is said needle-like MgCO 3
3. method according to claim 2 is characterized in that, said solubility magnesium salts is selected from MgCl 2, MgCl 26H 2O, MgSO 4Or MgBr 2In one or more.
4. method according to claim 3 is characterized in that the solubility magnesium salts is selected from anhydrous MgCl 2Or MgCl 26H 2O.
5. method according to claim 2 is characterized in that said alkali is selected from one or more in NaOH, KOH or the ammoniacal liquor.
6. method according to claim 2 is characterized in that, the volumetric molar concentration of the aqueous solution of alkali is 0.5mol/L～2.0mol/L.
7. method according to claim 2 is characterized in that, the mol ratio of solubility magnesium salts and alkali is: the solubility magnesium salts: alkali=1: 1～1: 1.2.
8. according to each described method of claim 1～7, it is characterized in that the length of fibrous light cakium carbonate is 10-80 μ m, length-to-diameter ratio is 20～80: 1.
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Publication number Priority date Publication date Assignee Title
CN101302026B (en) * 2008-06-30 2010-08-25 上海东升新材料有限公司 Honeycomb calcium carbonate, and preparation and application method thereof
CN101935865B (en) * 2010-09-08 2012-09-26 中国科学院青海盐湖研究所 Preparation method of high length-diameter ratio calcium carbonate whiskers
CN103539186A (en) * 2013-09-28 2014-01-29 昆山市周市溴化锂溶液厂 Preparation method of fusiform light calcium carbonate
CN105565355B (en) * 2014-10-13 2018-08-21 东升新材料（山东）有限公司 A kind of aragonitic fine particle calcium carbonate and its synthetic method for coating for paper
CN107034726A (en) * 2017-04-17 2017-08-11 华东理工大学 A kind of preparation method of dumb light paper coating calcium carbonate
CN110228986A (en) * 2018-12-13 2019-09-13 湖北工业大学 A method of promoting quick lime carbonization

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