CN102491395A - Preparation method of nano-grade calcium carbonate - Google Patents
Preparation method of nano-grade calcium carbonate Download PDFInfo
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- CN102491395A CN102491395A CN2011103729359A CN201110372935A CN102491395A CN 102491395 A CN102491395 A CN 102491395A CN 2011103729359 A CN2011103729359 A CN 2011103729359A CN 201110372935 A CN201110372935 A CN 201110372935A CN 102491395 A CN102491395 A CN 102491395A
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Abstract
The invention discloses a preparation method of nano-grade calcium carbonate. The invention belongs to the technical field of compound preparation. The method comprises steps that: S1, lime is digested; S2, a slurry obtained through digestion is sieved, and is then aged; S3, the aged slurry is carbonized; S4, the carbonized slurry is processed through primary cladding; S5, the slurry processed through primary cladding is subject to press-filtrating, drying, crushing, grading, and packaging, such that an intermediate product is obtained; S6, the intermediate product is subject to secondary cladding, such that a nano-grade calcium carbonate finished product is obtained. When the nano-grade calcium carbonate prepared with the method is used in RTV silicon rubber, the nano-grade calcium carbonate has both high dispersity and high reinforcing property.
Description
Technical field
The present invention relates to the preparing technical field of compound, particularly a kind of RTV Zylox that is exclusively used in possesses the preparation method of the nano-calcium carbonate of high reinforcement property and polymolecularity simultaneously.
Background technology
RTV Zylox is a kind of room temperture rubber vulcanization; Because it has high temperature resistant, low temperature resistant, moistureproof, insulation, performance such as ageing-resistant, and be applied to building, the silicone sealant in fields such as automobile, electronics, space flight, sun power, gather in the polymkeric substance such as sulphur glue, PVC glue.But the mechanical property of pure RTV Zylox is relatively poor, therefore, needs in the RTV Zylox to add reinforced filling, just can have use value.Common compensation filler is a WHITE CARBON BLACK, and lime carbonate uses as compatibilization filler in RTV Zylox.Along with the development of nanotechnology, calcium carbonate particles is the refinement trend development, and its crystalline structure and surface electronic structure also change; Formed nano-calcium carbonate; Compare with ordinary calcium carbonate, nano-calcium carbonate has quantum size effect, small-size effect, surface effects and macroscopic quantum effect, therefore; Nano-calcium carbonate also can be used as the reinforced filling of RTV Zylox; Because the price of nano-calcium carbonate is more cheap than the WHITE CARBON BLACK, so nano-calcium carbonate has broad application prospects in RTV Zylox.But the nano-calcium carbonate that prior art is produced is as reinforced filling the time, if do the particle diameter of nano-calcium carbonate little; Though reinforcement property has improved; But dispersed relatively poor, with the surface of the sealer of such nano-calcium carbonate production tiny particle is arranged, glossiness is not enough; If the particle diameter of nano-calcium carbonate is done greatly, though dispersiveness has improved, reinforcement property is relatively poor.
Summary of the invention
In order to address the above problem, to the present invention proposes and a kind ofly can produce the preparation method who has the nano-calcium carbonate of polymolecularity and high reinforcement property when being exclusively used in RTV Zylox.
The preparation method of nano-calcium carbonate provided by the invention may further comprise the steps:
S1: with lime slaking;
S2: after the postdigestive slurry of process sieves, with its slurry ageing;
S3: order is through the slurry carbonization after the ageing;
S4: the slurry to through carbonization once coats;
S5:, obtain intermediate product to carrying out press filtration → drying → pulverizing → classification → packing through the slurry that once coats;
S6: said intermediate product is carried out secondary coat, obtain the nano-calcium carbonate finished product.
As preferably, in the S1 process, the temperature of the water that is used to digest is 40~90 ℃, and the weight percent of water and lime is 5~10: 1.
As preferably, the S2 time length is 12~24h, in the S2 process, adds the crystal formation control agent, and addition is 0.4~1% of a lime butt weight.
As preferably, said crystal formation control agent is selected from EDTA, EDTA-Na
2, in the caster sugar, white sugar one or more.
As preferably, in the S3 process, TR is 20~30 ℃, and stirring velocity is 100r/min~150r/min, and adds dispersion agent, and addition is 0.4~1.6% of a lime butt weight.
As preferably, said dispersion agent is selected from one or more in potassium hydrogen phosphate, sodium hydrogen phosphate, trisodium phosphate, potassium pyrophosphate, vinylformic acid-2-acrylic amide-2-methyl propane sulfonic acid, vinylformic acid-Propylene glycol monoacrylate multipolymer, maleic acid-acrylic acid copolymer, the HPMA.
As preferably, in the S4 process, add coating, the addition of said coating is 2.4~4.8% of a calcium carbonate dry basic weight amount, and temperature is 60 ℃, and churning time is 2h.
As preferably, said coating is the mixture of longer chain fatty acid and modified silicon oil, and wherein, said modified silicon oil is selected from one or both in amino-modified silicone oil, phenyl silicone oil, hydroxy silicon oil, epoxide modified silicone oil, the carboxy-modified silicone oil.
As preferably, in the S6 process, add the secondary coating, said secondary coating addition is 1~4.6% of a calcium carbonate dry basic weight amount, and temperature is 60~120 ℃, and the time length is 15~45min.
As preferably, said secondary coating is a titanate coupling agent.
When the nano-calcium carbonate of using method preparation provided by the invention was used for RTV Zylox, nano-calcium carbonate had had polymolecularity and high reinforcement property simultaneously.
Embodiment
In order to understand the present invention in depth, the present invention is elaborated below in conjunction with specific embodiment.
Embodiment one
The lime that the limestone kiln calcining is good digests with 40 ℃ hot water; The weight proportion of water and lime is 10: 1, crosses strained pulp ageing 12 hours then, adds the crystal formation control agent in the ageing process; The kind of crystal formation control agent is EDTA, and addition is 0.4% of a lime solid content.The lime white that ageing is good is to 15m
3The special carbonization still of high speed shear carry out carbonization, carbonization temperature is controlled at 30 ℃, stirring velocity is 110r/min; The slurry that carbonization is good adds dispersion agent, and dispersion agent is sodium hydrogen phosphate, vinylformic acid-2-acrylic amide-2-methyl propane sulfonic acid multipolymer, and the addition of two kinds of dispersion agents respectively is 0.2% of a lime carbonate butt; Add sodium hydrogen phosphate earlier; Add vinylformic acid-2-acrylic amide-2-methyl propane sulfonic acid multipolymer after stirring 5min, sieve behind the restir 10min, to coating still.Its coating is cerinic acid CH
3(CH
2)
24COOH and amino-modified silicone oil, with sodium hydroxide saponification in the aqueous solution, saponification temperature is 80 ℃ with cerinic acid in elder generation, and the proportioning of water and cerinic acid is 100: 1, and the proportioning of cerinic acid and sodium hydroxide is 10: 1, behind 90 ℃ of saponification 30min, adds amino-modified silicone oil.The addition of amino-modified silicone oil is 1.2% of a lime carbonate butt, and the addition of cerinic acid is 1.2% of a lime carbonate butt, and the coating preparation was accomplished after the interpolation amino-modified silicone oil stirred 30min.The coating for preparing is put into 15m
3The coating jar in the nano-calcium carbonate slurry is stirred coating, temperature is 60 ℃, stirring the coating time is 120min.Coat good slurry and carry out press filtration, drying, pulverizing, classification, packing.The intermediate product that obtains carries out secondary at high mixer and coats, and the secondary coating is that sec.-propyl three (isostearoyl base) titanic acid ester, temperature of plate are 60 ℃, and the coating time is 45min, and addition is 4.6% of a lime carbonate butt.The technical indicator of the nano-calcium carbonate that makes at last is following:
Oil-absorption(number) % | Median size nm | Granule-morphology | Specific surface area m 2/g | The dispersed evaluation |
23 | 40 | Cubes | 44 | Good |
Embodiment two
The hot water digestion that the lime that the limestone kiln calcining is good is 50 ℃, the weight proportion of water and lime is 8: 1. cross strained pulp ageing 16 hours then, add the crystal formation control agent in the ageing process, the kind of crystal formation control agent is EDTA-Na
2, addition is 0.8% of a lime solid content.The lime white that ageing is good is to 15m
3The special carbonization still of high speed shear carry out carbonization, carbonization temperature is controlled at 26 ℃, stirring velocity is 120r/min; The slurry that carbonization is good adds dispersion agent, and dispersion agent is potassium hydrogen phosphate, vinylformic acid-Propylene glycol monoacrylate multipolymer, and the addition of two kinds of dispersion agents respectively is 0.4% of a lime carbonate butt; Add potassium hydrogen phosphate earlier, add vinylformic acid-2-acrylic amide-2-methyl propane sulfonic acid multipolymer behind the stirring 10min, sieve behind the restir 15min; To coating still, coating is xylogen acid CH
3(CH
2)
22COOH and phenyl silicone oil, with sodium hydroxide saponification in the aqueous solution, saponification temperature is 85 ℃ with xylogen acid in elder generation, and the proportioning of water and xylogen acid is 80: 1, and the proportioning of xylogen acid and sodium hydroxide is 11: 1, behind 95 ℃ of saponification 30min, adds phenyl silicone oil.The addition of phenyl silicone oil is 1.8% of a lime carbonate butt, and the addition of xylogen acid is 1.8% of a lime carbonate butt, and the coating preparation was accomplished after the interpolation phenyl silicone oil stirred 45min.The coating for preparing is put into 15m
3The coating jar in the nano-calcium carbonate slurry is stirred coating, temperature is 60 ℃, stirring the coating time is 120min.Coat good slurry and carry out press filtration, drying, pulverizing, classification, packing.The intermediate product that obtains carries out secondary at high mixer and coats, and the secondary coating is that sec.-propyl three (dioctyl pyrophosphoryl base) titanic acid ester, temperature of plate are 80 ℃, and the coating time is 30min, and addition is 3.4% of a lime carbonate butt.The technical indicator of the nano-calcium carbonate that makes at last is following:
Oil-absorption(number) % | Median size nm | Granule-morphology | Specific surface area m 2/g | The dispersed evaluation |
22 | 45 | Cubes | 40 | Good |
Embodiment three
The lime that the limestone kiln calcining is good digests with 70 ℃ hot water; The weight proportion of water and lime is 6: cross old 18 hours of strained pulp then 1.; Add the crystal formation control agent in the ageing process, the kind of crystal formation control agent is a caster sugar, and addition is 0.6% of a lime solid content.The lime white that ageing is good is to 15m
3The special carbonization still of high speed shear carry out carbonization, carbonization temperature is controlled at 24 ℃, stirring velocity is 130r/min; The slurry that carbonization is good adds dispersion agent, and dispersion agent is trisodium phosphate, maleic acid-acrylic acid copolymer, and the addition of two kinds of dispersion agents respectively is 0.6% of a lime carbonate butt; Add trisodium phosphate earlier, add maleic acid-acrylic acid copolymer behind the stirring 10min, sieve behind the restir 15min; To coating still, coating is cerinic acid C
22H
44O
2And amino-modified silicone oil, with sodium hydroxide saponification in the aqueous solution, saponification temperature is 90 ℃ with cerinic acid in elder generation; The proportioning of water and cerinic acid is 80: 1; The proportioning of cerinic acid and sodium hydroxide is 10: 1, behind 95 ℃ of saponification 30min, adds amino-modified silicone oil, and the addition of amino-modified silicone oil is 2.4% of a lime carbonate butt; The addition of cerinic acid is 2.4% of a lime carbonate butt, and the coating preparation was accomplished after the interpolation amino-modified silicone oil stirred 45min.The coating for preparing is put into 15m
3The coating jar in the nano-calcium carbonate slurry is stirred coating, temperature is 60 ℃, stirring the coating time is 120min.Coat good slurry and carry out press filtration, drying, pulverizing, classification, packing.The intermediate product that obtains carries out secondary at high mixer and coats, and the secondary coating is that two (dioctyl pyrophosphoryl bases) close fluoroacetic acid ester titanium, temperature of plate is 100 ℃, and the coating time is 20min, and addition is 2.2% of a lime carbonate butt.The technical indicator of the nano-calcium carbonate that makes at last is following:
Oil-absorption(number) % | Median size nm | Granule-morphology | Specific surface area m 2/g | The dispersed evaluation |
21 | 50 | Cubes | 37 | Good |
Embodiment four
The lime that the limestone kiln calcining is good digests with 90 ℃ hot water, and the weight proportion of water and lime is 5: 1. cross strained pulp ageing 24h then, add the crystal formation control agent in the ageing process, the kind of crystal formation control agent is a white sugar, and addition is 1% of a lime solid content.The lime white that ageing is good is to 15m
3The special carbonization still of high speed shear carry out carbonization, carbonization temperature is controlled at 20 ℃, stirring velocity is 150r/min; The slurry that carbonization is good adds dispersion agent, and dispersion agent is potassium pyrophosphate, HPMA, and the addition of two kinds of dispersion agents respectively is 0.8% of a lime carbonate butt; Add potassium pyrophosphate earlier, add HPMA behind the stirring 10min, sieve behind the restir 15min; To coating still, coating is xylogen acid and amino-modified silicone oil, and is earlier that xylogen is sour with sodium hydroxide saponification in the aqueous solution; Saponification temperature is 90 ℃, and the proportioning of water and xylogen acid is 80: 1, and the proportioning of xylogen acid and sodium hydroxide is 11: 1; Behind 95 ℃ of saponification 30min, add amino-modified silicone oil; The addition of amino-modified silicone oil is 2% of a lime carbonate butt, and the addition of xylogen acid is 2% of a lime carbonate butt, and the coating preparation was accomplished after the interpolation amino-modified silicone oil stirred 45min.The coating for preparing is put into 15m
3Cubical coats in the jar nano-calcium carbonate slurry is stirred coating, and temperature is 60 ℃, and stirring the coating time is 120min.Coat good slurry and carry out press filtration, drying, pulverizing, classification, packing.The intermediate product that obtains carries out secondary at high mixer and coats, and the secondary coating is that two (dioctyl pyrophosphoryl base) ethylene titanic acid ester, temperature of plate are 120 ℃, and the coating time is 15min, and addition is 1% of a lime carbonate butt.The technical indicator of the nano-calcium carbonate that makes at last is following:
Oil-absorption(number) % | Median size nm | Granule-morphology | Specific surface area m 2/g | The dispersed evaluation |
21 | 55 | Cubes | 32 | Good |
The preparation method of nano-calcium carbonate provided by the invention is dispersed into small bubble through high-speed stirring with dioxide gas, improves bubble quantity and bubble, increases the contact area of carbonic acid gas and calcium hydroxide; Also increase simultaneously the degree of supersaturation of carbanion and calcium ion in the solution; Quicken gas-liquid-solid three-phase rate of mass transfer, improve speed of response, in carbonization process; Through crystal formation control agent control crystalline size and pattern, keep the homogeneity of product pellet.Particulate carbon is combined to the coating that adds the back can control the lime carbonate surface electric charge, and improve sterically hindered, thereby make the nano-calcium carbonate of preparing method's preparation of adopting nano-calcium carbonate provided by the invention when being applied to RTV Zylox, possess polymolecularity.
Adopt the preparation method of nano-calcium carbonate provided by the invention because a large amount of calcium ions is contained on the lime carbonate surface; When coating, select for use and can lipid acid such as the cerinic acid of chemically combined long-chain, the wherein a kind of and modified silicon oil Combined Processing in the xylogen acid take place with lime carbonate surface calcium ion; The calcium ion generation chemical reaction that they can have with the lime carbonate surface; Thereby reduce the surface tension of lime carbonate; Reduce the secondary agglomeration in the pressure-filteration drying process; Middle product is carried out secondary with titanate coupling agent coat, can improve the bonding force between the organosilicon macromolecule in nano-calcium carbonate and the RTV Zylox, thereby make the nano-calcium carbonate of preparing method's preparation of adopting nano-calcium carbonate provided by the invention when being applied to RTV Zylox, possess high reinforcement property.
Above-described embodiment; The object of the invention, technical scheme and beneficial effect have been carried out further explain, and institute it should be understood that the above is merely embodiment of the present invention; Be not limited to the present invention; All within spirit of the present invention and principle, any modification of being made, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. the preparation method of a nano-calcium carbonate is characterized in that, may further comprise the steps:
S1: with lime slaking;
S2: after the postdigestive slurry of process sieves, with its slurry ageing;
S3: order is through the slurry carbonization after the ageing;
S4: the slurry to through carbonization once coats;
S5:, obtain intermediate product to carrying out press filtration → drying → pulverizing → classification → packing through the slurry that once coats;
S6: said intermediate product is carried out secondary coat, obtain the nano-calcium carbonate finished product.
2. method according to claim 1 is characterized in that, in the S1 process, the temperature of the water that is used to digest is 40~90 ℃, and the weight percent of water and lime is 5~10: 1.
3. method according to claim 1 is characterized in that, the S2 time length is 12~24h, in the S2 process, adds the crystal formation control agent, and addition is 0.4~1% of a lime butt weight.
4. method according to claim 3 is characterized in that, said crystal formation control agent is selected from EDTA, EDTA-Na
2, in the caster sugar, white sugar one or more.
5. method according to claim 1 is characterized in that, in the S3 process, TR is 20~30 ℃, and stirring velocity is 100r/min~150r/min, and adds dispersion agent, and addition is 0.4~1.6% of a lime butt weight.
6. method according to claim 5; It is characterized in that said dispersion agent is selected from one or more in potassium hydrogen phosphate, sodium hydrogen phosphate, trisodium phosphate, potassium pyrophosphate, vinylformic acid-2-acrylic amide-2-methyl propane sulfonic acid, vinylformic acid-Propylene glycol monoacrylate multipolymer, maleic acid-acrylic acid copolymer, the HPMA.
7. method according to claim 1 is characterized in that, in the S4 process, adds coating, and the addition of said coating is 2.4~4.8% of a calcium carbonate dry basic weight amount, and temperature is 60 ℃, and churning time is 2h.
8. method according to claim 7; It is characterized in that; Said coating is the mixture of longer chain fatty acid and modified silicon oil, and wherein, said modified silicon oil is selected from one or both in amino-modified silicone oil, phenyl silicone oil, hydroxy silicon oil, epoxide modified silicone oil, the carboxy-modified silicone oil.
9. method according to claim 1 is characterized in that, in the S6 process, adds the secondary coating, and said secondary coating addition is 1~4.6% of a calcium carbonate dry basic weight amount, and temperature is 60~120 ℃, and the time length is 15~45min.
10. method according to claim 9 is characterized in that, said secondary coating is a titanate coupling agent.
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CN110484023B (en) * | 2019-09-30 | 2021-05-14 | 建德市华宇纳米科技有限公司 | Preparation equipment and preparation method of high-dispersion nano calcium carbonate |
CN110791040A (en) * | 2019-11-01 | 2020-02-14 | 连州市凯恩斯纳米材料有限公司 | Nano calcium carbonate for toughening PVC (polyvinyl chloride) and preparation method thereof |
CN110791040B (en) * | 2019-11-01 | 2021-05-11 | 连州市凯恩斯纳米材料有限公司 | Nano calcium carbonate for toughening PVC (polyvinyl chloride) and preparation method thereof |
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